CONTENTS INSTRUCTIONS

NM-05640SP4
NM-05630SP3

4MM/3.2MM SOLID
SAMPLING SET

For the proper use of the instrument, be sure

to read this instruction manual. Even after you
read it, please keep the manual on hand so that
you can consult it whenever necessary.

INM-05640SP4-1
AUG2024-08521199
Printed in Japan
CONTENTS

NM-05640SP4
NM-05630SP3

4MM/3.2MM SOLID
SAMPLING SET

Please be sure to read this instruction manual carefully,

and fully understand its contents prior to the operation or
maintenance for the proper use of the instrument.
CONTENTS

NOTICE

・ This instrument generates, uses, and can radiate the energy of radio frequency and, if not installed and used in accordance
with the instruction manual, may cause harmful interference to the environment, especially radio communications.
・ The following actions must be avoided without prior written permission from JEOL Ltd. or its subsidiary company responsible
for the subject (hereinafter referred to as “JEOL”): modifying the instrument; attaching products other than those supplied by
JEOL; repairing the instrument, components and parts that have failed, such as replacing pipes in the cooling water system,
without consulting your JEOL service office; and adjusting the specified parts that only field service technicians employed or
authorized by JEOL are allowed to adjust, such as bolts or regulators which need to be tightened with appropriate torque.
Doing any of the above might result in instrument failure and/or a serious accident. If any such modification, attachment,
replacement or adjustment is made, all the stipulated warranties and preventative maintenances and/or services contracted
by JEOL or its affiliated company or authorized representative will be void.
・ Replacement parts for maintenance of the instrument functionality and performance are retained and available for seven
years from the date of installation. Thereafter, some of those parts may be available for a certain period of time, and in this
case, an extra service charge may be applied for servicing with those parts. Please contact your JEOL service office for
details before the period of retention has passed.
・ In order to ensure safety in the use of this instrument, the customer is advised to attend to daily maintenance and inspection.
In addition, JEOL strongly recommends that the customer have the instrument thoroughly checked up by field service
technicians employed or authorized by JEOL, on the occasion of replacement of expendable parts, or at the proper time and
interval for preventative maintenance of the instrument. Please note that JEOL will not be held responsible for any instrument
failure and/or serious accident occurred with the instrument inappropriately controlled or managed for the maintenance.
・ After installation or delivery of the instrument, if the instrument is required for the relocation whether it is within the facility,
transportation, resale whether it is involved with the relocation, or disposition, please be sure to contact your JEOL service
office. If the instrument is disassembled, moved or transported without the supervision of the personnel authorized by JEOL,
JEOL will not be held responsible for any loss, damage, accident or problem with the instrument. Operating the improperly
installed instrument might cause accidents such as water leakage, fire, and electric shock.
・ The information described in this manual, and the specifications and contents of the software described in this manual are
subject to change without prior notice due to the ongoing improvements made in the instrument.
・ Every effort has been made to ensure that the contents of this instruction manual provide all necessary information on the
basic operation of the instrument and are correct. However, if you find any missing information or errors on the information
described in this manual, please advise it to your JEOL service office.
・ In no event shall JEOL be liable for any direct, indirect, special, incidental or consequential damages, or any other damages of
any kind, including but not limited to loss of use, loss of profits, or loss of data arising out of or in any way connected with the
use of the information contained in this manual or the software described in this manual. Some countries do not allow the
exclusion or limitation of incidental or consequential damages, so the above may not apply to you.
・ This manual and the software described in this manual are copyrighted, all rights reserved by JEOL and/or third-party
licensors. Except as stated herein, none of the materials may be copied, reproduced, distributed, republished, displayed,
posted or transmitted in any form or by any means, including, but not limited to, electronic, mechanical, photocopying,
recording, or otherwise, without the prior written permission of JEOL or the respective copyright owner.
・ When this manual or the software described in this manual is furnished under a license agreement, it may only be used or
copied in accordance with the terms of such license agreement.

Copyright  2024 JEOL Ltd.

・ In some cases, this instrument, the software, and the instruction manual are controlled under the “Foreign Exchange and
Foreign Trade Control Law” of Japan in compliance with international security export control. If you intend to export any of
these items, please consult JEOL. Procedures are required to obtain the export license from Japan’s government.

TRADEMARK
・ Microsoft and Windows are either registered trademarks or trademarks of Microsoft Corporation in the United States and/or
other countries.
・ All other company and product names are trademarks or registered trademarks of their respective companies.

MANUFACTURER
JEOL Ltd. 3-1-2 Musashino, Akishima, Tokyo 196-8558, JAPAN
Telephone: 81-42-543-1111 Facsimile: 81-42-546-3353 URL: [Link]
Note: For servicing and inquiries, please contact your JEOL service office.
CONTENTS

WARRANTY
INFORMATION

1 Limited Warranty
Products manufactured by JEOL Ltd. (hereafter “JEOL products”) that fail under normal use by the
customer during the warranty period will be repaired or replaced, at JEOL’s discretion, without charge.
The components, modules and devices that are provided as replacements will be new parts or
refurbished parts that provide the same performance as new parts. All components, modules and
devices removed under this warranty become the property of JEOL.

1.1 Applicable Products

・ This warranty applies only to hardware and software products manufactured by JEOL Ltd.
・ For components that are not JEOL products, such as the computer, HDD, memory device, and the
like, the warranty provisions of the respective manufacturers shall apply.

1.2 Warranty Period

・ In the case of products for which the warranty period is recorded in the contract documentation, the
recorded warranty period shall take precedence.
・ If not specifically stated elsewhere, the warranty period is 12 months or a separately specified period
from the date on which the acceptance test is completed after delivery to the customer.
・ For components that are not JEOL products, like the computer, HDD, memory device, and the like,
the warranty start date shall be the date on which the acceptance test is completed after delivery to
the customer and the warranty periods established by the respective makers shall apply.
・ In the event that parts are replaced or repaired free of charge during the warranty period, there is no
change to the warranty start date or the warranty period for the product.

1.3 Scope of the Warranty

■Failure diagnosis
If a problem occurs, contact your JEOL service office and describe the conditions and content of the
problem. JEOL will assess the problem based on the situation and content of the problem.

■Repair method
If it is determined that the problem is caused by a fault or defect of a JEOL product, repair or
replacement will be performed free of charge. The choice of whether to repair or replace a component
is entirely at the discretion of JEOL.

■Warranty exclusions
This limited warranty does not extend to products for which any of the following situations apply. Even
within the warranty period, in the situations listed below, a fee will be charged to repair the product.
・ Product is operated or stored in an environment or under conditions that do not satisfy the specified
installation requirements.
・ The installation environment has changed (temperature, humidity, magnetic fields, etc.) since the
time of installation.
・ There is significantly accelerated deterioration of components and/or corrosion of electrical circuitry
as a result of exposure to extreme temperature, humidity, or an environment containing highly-
corrosive gases or excessive dust.
・ The quality of the utilities (including electricity, water, gas, air quality) has worsened.
・ The customer has relocated an installed instrument.
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・ Even in the case of a portable or movable instrument designed to be transported to a remote

location or moved around for use by the user, damage or failures caused during the instrument
relocation by the customer.
・ Product has not been properly maintained.
・ Consumable items or parts with the specified replacement period have not been replaced as
specified.
・ Corrupted operating system or application software, or damaged computer used with the instrument,
caused by shutting down the main power to the computer without performing the proper shutdown
sequence.
・ Products that have been disassembled, modified or repaired by the customer in ways other than
those specified in the instruction manuals provided with the instrument.
・ Products with damage or failure caused by using them in combination with hardware, software,
peripheral devices, and accessories that have not been provided or approved by JEOL.
・ Damage or failure resulting from a situation caused by the customer, such as failing to properly
manage the instrument, for which JEOL cannot be held responsible.
・ Corruption of the operating system or application software, or damage to a computer used with the
instrument, caused by fluctuations in the electricity or power failure.
・ Product damaged as a result of fire, earthquake, flooding, lightning or other natural disaster, or due
to local conflict or war.
・ Damage or malfunction of operating system, application software, or the instrument itself as a result
of infection by a computer virus.
・ Instruments that have been restored after being disposed of or re-sold without prior written notice to
and agreement from JEOL.

1.4 Items Not Covered by Warranty

・ Regardless of whether a product is still within the warranty period, this warranty does not cover
losses or damage to devices made by any other manufacturer at the customer site even if they are
damaged by a malfunction of the JEOL product.
・ JEOL is not responsible for any loss or damage to data recorded onto storage media, or to storage
units. The customer is responsible for making back-up copies of their own data.
・ Replacement parts for maintenance of the instrument functionality and performance are retained and
available for seven years from the date of installation. Thereafter, some of those parts may be
available for a certain period of time. Please contact your JEOL service office for details before the
period of retention has passed.
・ For items that are frequently updated, remodeled, or disappear from the market, like the computers
used with the JEOL products, it may not be possible to obtain an exact replacement.

2 Repairs for a Fee

Repairs of JEOL products are available with charges after the end of the warranty period, or at
anytime a customer requests. The components, modules and devices that are provided as
replacements during the paid repair work will be new parts or refurbished parts that provide the same
performance as new parts. All components, modules and devices removed during such repairs will
become the property of JEOL.
・ The warranty period for parts replaced and the service during paid repair work is a period of 3
months after the completion of the repairs; or, in the case of parts that must be periodically replaced,
the warranty period is the length of the specified replacement period.
・ In the event that repairs are performed again during the warranty period, there is no change to the
warranty start date or the warranty period.
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Notes on Disposal
for Business Users

Attention: ■ In the European Union

Your product is marked with
this symbol. It means that This symbol means that electrical and electronic equipment, at the
used electrical and electronic end of its life, should be disposed of correctly.
products should not be mixed In the European Union there is a separate collection system for used
with general household electrical and electronic products. Please help us to conserve the
waste. There is a separate environment we live in!
collection system for these
Electrical and electronic appliances and machines often contain
products.
materials which, if handled or disposed of incorrectly, are potentially
hazardous to human health and to the environment. They are,
however, essential for the correct functioning of your appliance or
machine. Therefore, please do not dispose of your old machine or
appliance together with your household waste.
Your JEOL product is designed and manufactured with high-quality
materials and components which can be recycled and reused. If the
product is used for business purposes and you want to discard it,
please contact your JEOL dealer, who will advise you about the end-
of-life disposal arrangements.

■ Outside the European Union

If you wish to discard this product, please contact your local
authorities and ask for the correct method of disposal.
CONTENTS

NOTATIONAL
CONVENTIONS AND
GLOSSARY
■ Examples for general notations

– CAUTION – : Important precautions for use, which, if not followed, may result in damage
to or problems with the device itself.
IMPORTANT NOTICES : Important notices for operating the instrument.
: Additional points to remember regarding the operation.

: A reference to another section, chapter or manual.

1, 2, 3 : Numbers indicate a series of operations to achieve a task.
◆: A diamond indicates a single operation that achieves a task.
File: The names of menus, commands, or parameters displayed on the screen
are denoted with bold letters.
File–Exit : Selecting a menu item from a pulldown menu is denoted by linking the menu
and the item with a dash (–).
For example, File–Exit means selecting Exit from the File menu.
Ctrl : Keys on the keyboard are denoted by enclosing their names in a box.

■ Examples for mouse and touch panel terminology

Mouse pointer: A mark, displayed on the screen, which moves following the movement of
the mouse. It is used to specify a menu item, command, parameter value,
and other items. Its shape changes according to the situation.
Click: To press and release the left mouse button.
Right-click: To press and release the right mouse button.
Double-click: To press and release the left mouse button twice quickly.
Drag: To hold down the left mouse button while moving the mouse.
Tap: Briefly touching and then releasing a point on a touch screen.
Double-tap: Tapping a point on a touch screen twice in rapid succession.
Swipe: Operation for changing the screen by touching a point on a touch screen and
dragging in a certain direction.
Pinch-in: Operation to reduce the image size on the screen by touching two points on
the touch screen simultaneously and dragging the two points closer
together.
Pinch-out: Operation to increase the image size on the screen by touching two points
on the touch screen simultaneously and dragging the two points farther
apart.
 CONTENTS

SAFETY PRECAUTIONS
PRECAUTIONS FOR USE
1 GENERAL ......................................................................................... 1
1.1 Outline .......................................................................................................... 1
1.2 Configuration................................................................................................ 1
2 DESCRIPTION OF PARTS ............................................................... 1
3 OPERATION ..................................................................................... 4
3.1 Notes on Handling Each Type of Sample ..................................................... 4
3.2 Assembling the Sample Tube (before Sampling) ......................................... 6
3.3 Notes on Sampling ....................................................................................... 8
3.4 How to Attach the Spinning Cap ................................................................ 11
3.5 Preparation for Spinning the Sample Tube ................................................. 13
3.6 Examples of Cap and Sleeve Failures ........................................................ 15
3.7 How to Remove the Caps ........................................................................... 16
3.7.1 Normal sample tube ................................................................................. 16
3.7.2 Heat-resistant sample tube and sealing sample tube ................................ 17
3.8 How to Take Out the Sample ...................................................................... 19
3.9 Examples of Failures .................................................................................. 20
4 MAINTENANCE .............................................................................. 22
4.1 Consumable Parts List ................................................................................ 22

NM-05640SP4-1
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Although this instrument is protected with safety device which

SAFETY
prevents the occurrence of accident that could result in an
injury, harm, and damage to the users or instrument itself, the
safety feature may not work properly if you use the instrument
for the purpose of use not intended or in an improper usage.
For the proper use of the instrument, please be sure to read all
PRECAUTIONS
of the instructions, descriptions, notices, and precautions
contained in this manual carefully to understand them fully prior Labels bearing the following symbols are
to the operation or maintenance. This section, “Safety attached to dangerous locations on the
Precautions”, contains important information related to safety for instrument. Do not touch any of these
using of the instrument. locations with your hands or anything else.
The safety indications and their meanings are as follows:

DANGER An imminently hazardous situation which, if not

avoided, will result in death or serious injury.
Beware of Beware of
electric shock laser
WARNING A potentially hazardous situation which, if not
avoided, could result in death or serious injury.

CAUTION A potentially hazardous situation which, if not Beware of Beware of

super low temp heat
avoided, may result in minor or moderate injury, or
a situation that could result in serious damage to
facilities or acquired data.

Beware of Beware of Do not

getting caught biohazard disassemble
Examples of symbols
Use the instrument properly within the scope of the purpose and usage described in its
brochures and manuals.
Never open/remove protective parts (exterior panels) and parts that can’t be
opened/removed without use of tool (including key), or disconnect/ connect the
cables/connectors that are not described in this manual.
Never attempt to do any works of disassembling/assembling the instrument other than
those described in this manual.
Never make modifications that include installing substitute parts and disabling safety
devices or other safety features.
Never disconnect the grounding wire or move it from the prescribed position. Failure to
follow this instruction could result in electric shock.
The AC power cord provided with this system is supplied for the particular device so
that never use it for any other equipment.
To avoid falling, do not climb onto the operation table and console during daily
operation or during maintenance or inspection.
When you dispose of the instrument or liquid or other waste, follow all applicable laws
and regulations, and dispose of it in a proper manner without polluting the environment.
Be sure to read the “Safety Precautions” section of the manuals for the accessories
attached to or built into the instrument.
If anything is unclear, please contact your JEOL service office.

WARNING for Installation

Do not attempt to install the instruments by yourself.
Installation work requires professional expertise and JEOL is responsible for the
installation of the instruments and related attachments purchased from JEOL.
Consult your JEOL service office.

NM-05640SP4-1 S-1
CONTENTS

CAUTION
• Do not insert samples that may ignite or explode due to high temperature,
impact, or pressure.
The sample tube may break into pieces and cause injury.
• Be careful of frostbite when using cooling gas.

Safety Instructions for Using JEOL Products

• Products using materials hazardous for operators or equipment
When measuring, indicating, or detecting harmful or corrosive substances, or voltages or other
electrical quantities that may cause electric shock, read the instruction manual carefully to assure
proper operation. Ensure that all operators of the instrument receive training on the operation
method.
If there is a problem in the product, take appropriate measures in accordance with the instruction
manual and contact a JEOL service office immediately.
• Products having accessible parts that reach high temperatures
If an accessible part of the product reaches a high temperature while it functions, notify all the
operators to exercise cautions whenever they will be near any such parts.
It is recommended to take measures to restrict the access to the instrument by enclosing with
rope or chain.
Do not use a chain made from magnetic materials near nuclear magnetic resonance (NMR)
instruments or electron spin resonance (ESR) instruments.
• Using JEOL product for an integrated system with other manufacturer’s product
Consult your JEOL office. We assume no responsibility for any damages resulting from using
the product in combination with other manufacturer’s product without consultation.
• Using product in an environment that does not satisfy the installation
requirements
Consult your JEOL office. We assume no responsibility for any damages resulting from using
the product in an environment other than one specified by JEOL without consultation.
• Attachment used for JEOL product
For safety reasons, only use the accessories or attachments that are supplied or designated by
JEOL. We assume no responsibility for any damages resulting from using any accessory or
attachment other than those specified by JEOL.
Do not replace detachable main power supply cords with inadequately rated cords.

S-2 NM-05640SP4-1
 CONTENTS

The following precautions are important which, if not followed,

PRECAUTIONS
may result in damage to the instrument itself.

FOR USE

• Normal and heat-resistant sample tubes are designed for solid-state samples only.
These products do not guarantee highly airtightness for liquid or gel samples.
If these sample tubes are used, the sample may leak from the sample tube, causing a spinning
error and probe damage.
• Do not rub the marking on the bottom cap for spinning detection with a cloth or
gauze.
If the marking is rubbed off, it may cause a spinning error and damage the sample tube or probe.
• When inserting the cap into the sleeve, do not hit the cap with a hard object.
The cap may become deformed, resulting in a spinning error.
• Do not use the sample tube with contamination adhering to it.
If you spin the sample tube with sample or dirt adhering to its surface, the inside of the spinner
will become contaminated, causing a spinning error. Additionally, when wiping the bottom cap,
be careful not to remove the marking on the surface.
• Be careful not to damage the turbine flutes of the spinning cap or touch the
marking with the blade edges of the cap tweezers.
Damaging the turbine flutes may result in a spinning error.
If the marking comes off, it may cause a detection error.
• Do not use the sampling stick when removing the spinning cap or bottom cap.
Damaging the caps may result in a spinning error.
• Do not damage the cap with the blades of the cap tweezers.
If you try to hold the boundary between the sleeve and the cap with the cap tweezers from the
beginning, it will damage the cap and cause a spinning error.
In addition, scratches on the cap may increase during sample tube spinning and cause the sample
tube to break.
• When removing the caps of heat-resistant sample tubes or sealing sample tubes,
be sure to cool the caps sufficiently.
If you forcibly pull out the cap without cooling it, the cap or tweezers may become damaged.
In addition, scratches on the cap may increase during sample tube spinning. This may cause the
sample tube to break and result in probe failure.
• Do not use liquid nitrogen.
If you use liquid nitrogen, the thermal shock may weaken the sleeve (cylinder).
This may cause the sleeve to break while the sample tube is spinning.
The temperature of liquid nitrogen (-196 ℃) causes rapid thermal contraction. This may cause
the sleeve to crack.
• When attaching or detaching the caps of heat-resistant sample tubes or sealing
sample tubes, be sure to use a cooling spray to cool the caps sufficiently.
Cooling causes the caps to thermally contract, making them easier to be attached and detached.
If the caps are not detached or fit after one cooling, cool them again.
• If you forcibly press the cap into the sleeve without cooling it, the sleeve may
crack due to the wedge effect.
Even if there are no visible cracks in the sleeve, fine cracks may occur, which increases the
possibility of the sample tube breaking while spinning at high speed and causing a probe failure.
• Keep this product in clean condition without any dirt or dust.
Dirt or dust adhering to the sample tube can cause spinning errors and prevent accurate sample
measurements.
• If there are any scratches, deformation, or abrasion of this product, consult your
JEOL service office.
This may cause the product to not perform as expected and accurate sampling may not be
possible.

NM-05640SP4-1 P-1
 CONTENTS

1 GENERAL
1.1 Outline
The NM-05640SP4 4MM/3.2MM Solid Sampling Set is a tool for loading and scraping the
samples for a solid object sample tube.

1.2 Configuration
Solid sampling set .............................................................................................. 1 set
Description:
Storage case .................................................................................................... 1
Cap tweezer .................................................................................................... 1
Sample packing parts...................................................................................... 1 set
Description:
Holder ......................................................................................................... 1
Support ....................................................................................................... 1
Support ....................................................................................................... 1
Sample scraper ............................................................................................... 1
Sampling stick ................................................................................................ 1
Needle with handle ......................................................................................... 1
Instruction manual .............................................................................................. 1

2 DESCRIPTION OF PARTS
■ Storage case

Dedicated storage case for the solid sampling kit.

Figure 1 Storage case

NM-05640SP4-1 1
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■ Sampling stick

The gauge that is pressed against the sample to measure the sample amount when filling
the sample tube with the sample.

Figure 2 Sampling stick

■ Sample scraper

Used to scrape the sample out of the sample tube to adjust the sample amount.

Figure 3 Sample scraper

■ Sample packing parts

When filling the sample tube with the sample, the sample tube is set in the center of the
holder, and when combined with the sample loading support, it is used as a guide to
smoothly introduce the sample. In addition, when combined with the holder and the cap
closing support, it is used as a guide to close the cap of the sample tube.
Sample loading Cap closing
support support

Holder

Bottom
cap

Bottom
cap

Figure 4 Sample packing parts

2 NM-05640SP4-1
 CONTENTS

■ Cap tweezers

Used for removing the caps of the sample tube. The cap can be removed easily by aligning
the blade edge to the boundary between the cap and the sleeve and then gripping the
tweezers firmly. The removed cap fits inside the protective plate, making it difficult to lose.

Figure 5 Cap tweezers

■ Needle with handle

The spacer can be taken out of the sleeve by inserting the tip of this needle into the hole at
the center of the spacer.

Figure 6 Needle with handle

NM-05640SP4-1 3
CONTENTS

3 OPERATION
The following procedure requires powder-free rubber gloves and a cooling spray. They are
not supplied with the product and must be prepared by the customer.

3.1 Notes on Handling Each Type of Sample

■ Powder sample

Mix the powder as evenly as possible using an agate mortar.

■ Block-shaped sample

● Rubber, etc.
Chop the sample as fine as possible, ideally 1 mm3.
 A craft knife is convenient for such fine processing.

You can also process the sample into a cylindrical shape that fits the inner diameter of
the sleeve.
 Spacers help spinning become stable.
Large sample pieces Fine sample pieces Cylindrical sample

Spacer Spacer Spacer

Figure 7 Block-shaped sample

 If the particle diameter of the sample piece is large, there is more space in the
sample tube.
 If you spin the sample tube in this state, the centrifugal force may make the
sample uneven.
 If the sample becomes uneven, the spinning control may become unstable.

4 NM-05640SP4-1
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■ Film-shaped sample

● Method 1: Rolling

Roll the film while Insert the film into

making the top flat. the sample tube.
Figure 8 How to roll the film

● Method 2: Stacking

Spacer
Chop into fine Stack the
pieces. pieces.

Figure 9 How to stack film sample pieces

■ Liquid or gel sample

Use airtight products such as a sealing sample tube for a liquid or gel sample. Avoid
normal or heat-resistant sample tubes.

―CAUTION―
Normal and heat-resistant sample tubes are designed for solid-state
samples only. These products do not guarantee highly airtightness for
liquid or gel samples.
If these sample tubes are used, the sample may leak from the sample tube, causing a
spinning error and probe damage.

NM-05640SP4-1 5
CONTENTS

3.2 Assembling the Sample Tube (before Sampling)

CAUTION
Do not insert samples that may ignite or explode due to high
temperature, impact, or pressure.
The sample tube may break into pieces and cause injury.

1. Insert the bottom cap into the sleeve (Figure 10) by using the holder and cap
closing support of the sample packing parts (Figure 4).
Insert the cap without forming a gap.
 Either end of the sleeve can be top or bottom.

Bottom cap

Sleeve

Figure 10 Sleeve with the bottom cap inserted in it

―CAUTION―
• Do not rub the marking on the bottom cap for spinning detection
with a cloth or gauze.
If the marking is rubbed off, it may cause a spinning error and damage the
sample tube or probe.
• When inserting the cap into the sleeve, do not hit the cap with a
hard object.
The cap may become deformed, resulting in a spinning error.

■ Merits of using spacers

The spacers are effective for stabilizing the spinning of the solid object sample tube.
Sampling with a small amount of sample can be performed.
 If no spacer is used
The sample may enter the inside of the spinning cap and the bottom cap.
In particular, if the sample enters the inside of the spinning cap, the compression of
the sample that was loaded evenly is degraded. As the sample becomes more spread,
the spinning of the sample tube may become unstable.
We recommend using spacers as much as possible.

6 NM-05640SP4-1
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After sampling During sample When spacers

tube spinning are used

The sample enters the inside

of the spinning cap.
This degrades the
compression status of the
sample in the sleeve.

Spacer

The sample enters the

inside of the bottom cap.

Figure 11 Spacers

1. Insert a spacer into the sleeve as necessary (Figure 12).

When no spacer is required, proceed to the next step.
Spacer

Figure 12 Sleeve with a spacer inserted

2. Set the sample tube prepared at step 1 into the holder of the sample packing
parts so that the holder and the sample loading support are assembled (Figure
4).
Set the sample tube with the bottom cap facing downward as shown in Figure 13.

Sample packing parts

(Holder and sample Sleeve
loading support)

Sample

Bottom cap Spacer

Figure 13 Sample packing parts attached to the sample tube

NM-05640SP4-1 7
CONTENTS

3.3 Notes on Sampling

■ Do not load a large amount of sample at once

If you load a large amount of sample into the sleeve at once, the sample is likely to become
uneven. Add the sample gradually.
• The amount of sample to be inserted each time
3.2 mm/4 mm 8 mm sample
Overloaded
sample tube tube

1/2 of laborator y 1 of laborator y

Laboratory spatula spatula spatula

Figure 14 The amount of sample to be loaded each time

1. The sample must be approximately 1 mm high in the sample tube.
2. Press the sample with the sampling stick (Figure 15).
Avoid applying excessive force.
 If pressed excessively, the sampling stick may become deformed.
Sampling
stick

Sample
Sample packing parts
(Holder and sample Spacer
loading support)

Figure 15 Sampling stick

 Do not shake the sampling stick horizontally (Figure 16).

This may deform the sampling stick or break the sleeve.
Do not shake the stick horizontally.

Figure 16 Do not shake the sampling stick horizontally

3. Repeat steps 1 to 2.

8 NM-05640SP4-1
 CONTENTS

4. Adjust the sample amount by using the sampling stick (Figure 17).
It is very difficult to adjust the sample amount exactly at the specified height. A height
slightly lower than that will be acceptable.
When taking out the sample, use the needle with handle or a sample scraper (Figure
18).

Guidelines for filling the sample

tube with the sample
With spacer for
heat-resistant
With spacer sample tube

Without spacer

Figure 17 Guidelines for loading the sample by using the sampling stick

Needle with Sample scraper

handle

Figure 18 Needle with handle and sample scraper

 If the sample is overloaded, it may cause errors such as the spinning cap coming
off during the spinning of the sample tube (Figure 19).
 In such cases, decrease the sample amount.
Not correct Not correct
Correct

With slightly smaller With appropriate When the sample

amount of sample amount of sample is overloaded

Sample

Figure 19 Adjusting the sample amount

NM-05640SP4-1 9
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■ Errors caused by overloading the sample

If the sample is overloaded into the solid object sample tube, the cap may not be firmly
attached.
If the sample spinning is performed while the cap is not firmly attached, the cap may come
off during spinning, which may cause a probe failure.

In particular, on the solid-state NMR system, by spinning the sample tube at a high rate, the
temperature of the sample itself rises.
Temperature rise

Spinning rate

Figure 20 Example of a temperature calibration curve sample tube.

Normally, as the sample temperature rises, the sample volume increases due to thermal
expansion.
The thermal expansion coefficient is different according to the type of sample. In addition
to the thermal expansion of the sample, if the sample is overloaded, the cap is pressed
upward. This may cause the cap to come off.
Therefore, it is better to load a slightly smaller amount of sample into the solid object
sample tube than the standard amount.
Even if the sample amount decreases slightly, the sensitivity does not significantly
decrease.

Thermal expansion
Glass < metal <<< resin
Metal has an thermal expansion rate four times that of glass, while resin has an
thermal expansion rate 20 to 30 times that of glass.

Check there is no gap. Check there is no gap.

Figure 21 Sample tube

10 NM-05640SP4-1
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3.4 How to Attach the Spinning Cap

■ Inserting a spacer

 Insert a spacer and check the height.

Correct Not correct Not correct

With
With slightly appropriate When the
smaller amount amount of sample is
of sample sample overloaded

Spacer

Sample

Figure 22 Adjusting the sample tube height with a spacer

■ Normal sample tube

 Attach the spinning cap to the sleeve by using the sample packing parts
(holder and cap closing support).

■ Heat-resistant sample tube and sealing sample tube

1. Sufficiently cool down the spinning cap with cooling gas (Figure 23).
 Provide sufficient cooling by spraying cooling gas for 30 to 40 seconds.
CAUTION
Be careful of frostbite when using cooling gas.

NM-05640SP4-1 11
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2. Quickly attach the cooled spinning cap to the sleeve by using the sample
packing parts (holder and cap closing support).
 If the cap cannot be inserted smoothly, cool the cap again.
 Do not forcibly push the cap inward.

Cooling gas nozzle If the cap cannot be inserted

smoothly, cool the cap again.

Figure 23 Cooling the spinning cap

 Avoid pressing the table or the like with the cap to forcibly insert it into the
sleeve (Figure 24).
This may deform the spinning cap or damage the sleeve.

Table Cap

Figure 24 Avoid pressing the table with the cap

12 NM-05640SP4-1
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3.5 Preparation for Spinning the Sample Tube

1. Closely attach the cap.
 If the sample is overloaded, it becomes difficult to attach the cap (Figure 25).
 Check that there is no gap between the sleeve and caps of the sample tube
(Figure 26).

Figure 25 Gap between the sleeve and caps of the sample tube

Check there is no gap. Check there is no gap.

Figure 26 Sample tube
2. Check the marking.
a. Allow the black marking to dry for at least 30 minutes.
If it is not completely dry, part of the marking will be scratched off due to a
centrifugal force and contaminate the spinning detection part, causing spinning
detection malfunction.
 In particular, the gold marking of the sealing sample tube takes much time to dry.
In some cases, it may take a whole day to completely dry.
If the sample tube is used before the marking is completely dry, the marking will
be scratched off and contaminate the probe.
b. Apply the marking appropriately (Figure 27).
 If the marking adheres to the sleeve, it may cause wrong recognition of the
spinning rate or a spinning error.
 If the marking adheres to the bottom surface, the marking acts as an adhesive and
causes a spinning error.

Marking inappropriately applied

and adhering to the sleeve.

Marking inappropriately applied to

the bottom surface of the bottom cap.
Figure 27 Marking inappropriately applied

NM-05640SP4-1 13
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3. Check that the sleeve is not damaged (Figure 28).

 There may be a crack on the sleeve. If such a sample tube is used, the sample
tube may break into pieces during spinning.

Figure 28 Scratches on the sleeve

4. Check that the cap is not deformed.
 Check that the turbine flutes on the spinning cap are not deformed.
 Check that the bottom cap is not deformed.
5. Wear powder-free rubber gloves when handling the completed sample tube
unit and remove any contamination.
 Clean the surface of the sample tube using a wipe or similar.
 Wipe off skin oil.
 Wipe off the sample adhered to the cap.

―CAUTION―
Do not use the sample tube with contamination adhering to it.
If you spin the sample tube with sample or dirt adhering to its surface, the inside
of the spinner will become contaminated, causing a spinning error.
Additionally, when wiping the bottom cap, be careful not to remove the
marking on the surface.

14 NM-05640SP4-1
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3.6 Examples of Cap and Sleeve Failures

Cap/sleeve condition Factors for failure Actions to take

Cap deformed ・ The sample tube and the probe ・ Replace the spinning cap.
cover collided or made other ・ Replace the bottom cap.
contact due to the protrusion
of the sample tube.
・ Excessive force was applied to
the cap when it was inserted.
・ The turbine flutes of the ・ Replace the spinning cap.
Spinning cap deformed spinning cap were deformed or
partly lost.
・ The spinning cap has become
degraded or worn out, or it
was deformed when it was
inserted.
Spinning cap deformed ・ Damaged by the cap tweezers. ・ Replace the spinning cap.

Cap insertion failure ・ The sample is overloaded. ・ Perform sampling again.

・ The sample is not uniformly ・ Replace the spinning cap.
loaded.
・ The spinning cap is deformed.

Cap insertion failure ・ The sample is overloaded. ・ Perform sampling again.

・ The spinning cap is loose. ・ Replace the spinning cap.

・ There are scratches on both ・ Perform sampling again.

Scratches on the sleeve
ends of the sleeve. ・ Depending on the depth of
・ The spinning error of the the damage, the sleeve must
sample tube caused the sample be replaced.
tube to contact the sleeve.
・ The sample is loaded wrongly
and causes a spinning error.
Scratch on the sleeve ・ There is a scratch on the ・ Replace the spinning cap.
middle part of the sleeve. ・ Replace the bottom cap.
・ The sample tube popped out ・ Depending on the depth of
and collided with the stator. the damage, the sleeve must
be replaced.
・ Repair the probe.

NM-05640SP4-1 15
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3.7 How to Remove the Caps

―CAUTION―
• Be careful not to damage the turbine flutes of the spinning cap or touch
the marking with the blade edges of the cap tweezers.
Damaging the turbine flutes may result in a spinning error.
If the marking comes off, it may cause a detection error.
• Do not use the sampling stick when removing the spinning cap or
bottom cap.
Damaging the caps may result in a spinning error.

3.7.1 Normal sample tube

1. Lightly hold the sleeve of the sample tube with the blades of the cap tweezers
(Figure 29).

Cap tweezers blade

Sleeve

Figure 29 Sleeve and cap tweezers blades

2. By sliding the sleeve, the blades are inserted into the boundary between the
sleeve and the cap (Figure 30).

Slide the sleeve

Figure 30 Sliding and inserting the blades into the boundary between the sleeve and the cap
3. Grip the cap tweezers (Figure 5) firmly (Figure 31).
Check that the blades have been completely closed (①) and there is a gap between the
spinning cap and the sleeve (②).
①

Figure 31 Removing the caps

16 NM-05640SP4-1
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4. Pull out the cap while holding the sample tube firmly (Figure 32).
 Pull the cap tweezers without tilting them.
 If the sample tube is slippery, wear rubber gloves or similar to hold it (with the
sleeve).

Figure 32 Pulling out the caps

―CAUTION―
Do not damage the cap with the blades of the cap tweezers.
If you try to hold the boundary between the sleeve and the cap with the cap tweezers
from the beginning, it will damage the cap and cause a spinning error.
In addition, scratches on the cap may increase during sample tube spinning and
cause the sample tube to break.

3.7.2 Heat-resistant sample tube and sealing sample tube

1. Be sure to spray cooling gas for 30 to 40 seconds to cool down the cap
sufficiently (Figure 33).
 Cooling spray PN: 780258185, etc.

Cooling spray

Figure 33 Cooling the caps

2. Quickly hold the sleeve of the sample tube with the cap tweezers blades
(Figure 34).
 Avoid holding the boundary between the cap and the sleeve from the beginning.

Cap tweezers blade

Sleeve

Figure 34 Sleeve and cap tweezers blades

NM-05640SP4-1 17
CONTENTS

3. By sliding the sleeve, the blades are inserted into the boundary between the
sleeve and the cap (Figure 35).

Slide the sleeve

Figure 35 Sliding and inserting the blades into the boundary between the sleeve and the cap
4. Grip the cap tweezers (Figure 5) firmly (Figure 36).
Check that the blades have been completely closed (①) and there is a gap between the
spinning cap and the sleeve (②).
①

Figure 36 Removing the caps

5. Pull out the cap while holding the sample tube firmly (Figure 37).
Pull the cap tweezers without tilting them.
 If the sample tube is slippery, wear rubber gloves or similar to hold it (with the
sleeve).

If the cap cannot be pulled out, cooling was not performed sufficiently.
 In that case, cool the cap by using the cooling spray sufficiently, and then pull
out the cap.

Figure 37 Pulling out the caps

―CAUTION―
• When removing the caps of heat-resistant sample tubes or sealing
sample tubes, be sure to cool the caps sufficiently.
If you forcibly pull out the cap without cooling it, the cap or tweezers may become
damaged. In addition, scratches on the cap may increase during sample tube
spinning. This may cause the sample tube to break and result in probe failure.
• Do not use liquid nitrogen.
If you use liquid nitrogen, the thermal shock may weaken the sleeve (cylinder).
This may cause the sleeve to break while the sample tube is spinning.

18 NM-05640SP4-1
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3.8 How to Take Out the Sample

1. Remove the spinning cap by referring to Section 3.7 "How to Remove the Caps".
2. Take out the spacers by using the needle with handle (Figure 38).
Slightly insert the needle with handle into the hole of the spacer, and then slowly take
it out of the sleeve.
Be careful not to insert the needle too far into the spacer, as this can widen the hole in
the spacer.

Figure 38 Needle with handle

3. Loosen the sample gradually by using the needle with handle to take it out
(Figure 39).
Even if you use a sample scraper from the beginning, it is difficult to take out the
sample.
Use the sample scraper only after taking out a certain amount of sample.
Spacer

Bottom cap Sample Needle with handle

Step 1. Scrape the sample out of the tube by using the needle with handle.

Step 2. After removing most of the sample, use the sample scraper.

Figure 39 Taking out the sample

4. Clean the entire sleeve by using a wipe.
Clean the sample tube sleeve, spacers, and caps with water or ethanol.
 Avoid using other solvents than water and ethanol because they may deform or
degrade the parts.
5. Remove the bottom cap by using the cap tweezers (Figure 5).
Remove the bottom cap by the same method as described in Section 3.7.
6. Take out the spacer with the sampling stick (Figure 2).
Press the spacer out of the sleeve by using the sampling stick.
7. Clean and store the sleeve, spacer, and caps.
 The fit of the caps and sleeves varies for each set, so store them in the sets as
they were shipped.

NM-05640SP4-1 19
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3.9 Examples of Failures

■ Scratches on Caps

Figure 40 is an image of the cap with a scratch which was made with the cap tweezers
when the spinning cap and bottom cap were pulled out of the sleeve.
The deformation of the cap may cause a spinning error of the solid object sample tube.
Either cap may become damaged during high-speed spinning of the sample tube and cause
a probe failure.

Scratch made with cap

tweezers blade

Figure 40 Scratch on the cap

■ Heat-resistant sample tube and sealing sample tube

● Cooling spray
Figure 41 is an image of the cap with a scratch which was made with the cap tweezers
when the spinning cap and bottom cap were forcibly pulled out of the sleeve.

Cap tweezers blade

Spinning cap

Sleeve

Worn blades

Scratch made with cap tweezers blade

Figure 41 Example of a damage

20 NM-05640SP4-1
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―CAUTION―
• When attaching or detaching the caps of heat-resistant sample tubes or
sealing sample tubes, be sure to use a cooling spray to cool the caps
sufficiently.
Cooling causes the caps to thermally contract, making them easier to be attached and
detached.
If the caps are not detached or fit after one cooling, cool them again.
• If you forcibly press the cap into the sleeve without cooling it, the sleeve
may crack due to the wedge effect.
Even if there are no visible cracks in the sleeve, fine cracks may occur, which
increases the possibility of the sample tube breaking while spinning at high speed
and causing a probe failure.
• Do not use liquid nitrogen.
The temperature of liquid nitrogen (-196 ℃) causes rapid thermal contraction. This
may cause the sleeve to crack.

NM-05640SP4-1 21
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4 MAINTENANCE
―CAUTION―
• Keep this product in clean condition without any dirt or dust.
Dirt or dust adhering to the sample tube can cause spinning errors and prevent
accurate sample measurements.
• there are any scratches, deformation, or abrasion of this product,
If
consult your JEOL service office.
This may cause the product to not perform as expected and accurate sampling may
not be possible.

4.1 Consumable Parts List

The parts shown in the table below are consumables. If any one of them is damaged during
use, contact the JEOL sales or service office to place an order.
Part name Part number Description
Holder 822381796 (for 3.2 mm Included in the sample
sample tube) packing parts.
822382172 (for 4 mm)

Support 822381851 (for 3.2 mm) Sample loading support,

822382181 (for 4 mm) included in the sample
packing parts.

Support 822381877 (for both 3.2 Cap closing support,

mm and 4 mm) included in the sample
packing parts.

Sampling stick 822381885 (for 3.2 mm) Tip part of the sampling
(resin) 822382199 (for 4 mm) stick.
The resin type
(polyoxymethylene) is the
same as the standard item
supplied with the product.
Sampling stick (For 3.2 mm) Tip part of the sampling
(metal) (For 4 mm) stick.
The metal type (stainless
steel) may damage the
sample tube.
It is suitable for use by
experts.
Drill for solid 420006681 (for 3.2 mm) Tip part of the sample
objects 420006711 (for 4 mm) scraper.
Plate 820467642 (for 3.2 mm) Cap tweezers blade.
820468193 (for 4 mm)

Needle with 424012154

handle

22 NM-05640SP4-1