Sample Preparation Service

Contents

1. Service Overview
2. Category of Service
3. Fees
4. Sample Conditions
5. Usage Procedures
6. Post-Implementation Processes
7. Contacts

1. Service Overview

Sample Preparation Service is a fee-based service in which samples sent in advance by users are prepared by the staff of the Japan Synchrotron Radiation Research Institute (JASRI) and are available in the form of finished preparations at the time of the experiment. This service is available regardless of the type of proposal. However, please contact us for graduate student proposals.

2. Category of Service

• Powder capillary filling for powder diffraction experiment (BL02B2, BL13XU)
• Pellet preparation for XAFS experiment (BL01B1, BL14B2)

3. Fees

After the beamtime, the fee will be calculated based on the amount of sample preparation service used and will be billed accordingly.

4. Sample Conditions

【Common to both Powder diffraction and XAFS】Specific chemical substances will not be accepted during the 2025B term.

【Powder diffraction（BL02B2, BL13XU）】

• Powder samples will be automatically filled into capillaries.
• Only samples consisting of particles sufficiently smaller than the capillary diameter and stable in air are acceptable.
• Capillaries should be selected from borosilicate glass or quartz, with outer diameters of either 0.3 mm or 0.5 mm.
• Please prepare the powder sample in the sample vial specified below:
  9-852-01 LABORAN Screw Tube Bottle 2mL
  https://axel.as-1.co.jp/asone/d/9-852-01/
  * The minimum required powder amount is approximately 10 scoops with a spatula (approx. 20 mg).
• Please pack the vial in the dedicated case that will be sent to you later.
  Ensure that no powder adheres to the outside of the vial or inside the case.
  Avoid affixing tape to the vial. Please write necessary information directly on the vial with a marker if you need.

NOTE

• – Samples that are unstable in air, toxic or hazardous, or contain particles larger than the capillary diameter are not accepted.
• – Only ambient atmosphere and room temperature conditions are supported. We cannot accommodate air-sensitive handling or temperature control.
• – Depending on the physical characteristics of the powder, proper filling into the capillary may not be achieved.
• – This service (powder capillary filling) does not guarantee successful XRD data acquisition or data quality.

【XAFS（BL01B1, BL14B2）】

• Pellets are prepared by mixing the sample and boron nitride (BN) powder.
• Samples must be in powder form, with a particle size of approximately 2 µm or less and be stable in air.
• Sample powder should be sealed in the following sample tube bottles.
  　　Sample-Tube bottle : Clear 5 mL No.2 (inner diameter x cylinder diameter × Total length: φ13 × φ18 × 40 mm)
  　　[Maruemu Corporation] Order No. 5-096-04
• Refer to the following manual and programme to estimate and weigh the sample powder required for measurement by the transmission mode.
  * Sorry, the manual and programme are only available in Japanese.
  　　Automatic Pellet Sample Preparation System for XAFS Measurement:　Manual of sample preparation procedures
  　　XAFS sample preparation guide programme
• Minimum Order Quantity is 10 pellets.
• Taking into account variations in sample powder weighing accuracy, etc., it is recommended that at least three pellets are prepared per level.
• In addition to the pellets produced, waste (e.g. sample tube bottles, bentcot from stirring and compression rod cleaning) must also be picked up.

NOTE

• – Samples that are unstable under atmospheric conditions, have non-uniform particle size, are toxic or require large quantities for pelleting are excluded.
• – This service is for atmospheric room temperature environments. Handling of non-atmospheric exposure, temperature control, etc. is not covered.
• – This service (sample pellet preparation) does not guarantee the availability or quality of XAFS measurement data.

【Common to both Powder diffraction and XAFS】

Unacceptable Sample

The following samples are not accepted:
a) Biological samples (e.g. animals, plants, and microorganisms)
b) “Level 4” chemicals defined by JASRI (i.e. substances requiring the approval of the competent authority)
– Specific substances regulated by the “Law on the Prohibition of Chemical Weapons and the Regulation of Specific Chemicals”
– Narcotic and psychotropic drugs regulated by the “Narcotics and Psychotropics Control Law”
– Stimulant drugs and ingredients of stimulant drugs regulated by “Stimulant Drug Control Law”
– Hemp and hemp products regulated by the “Cannabis Control Law”
– Opium, poppy or poppy straw regulated by the “Opium Law”
– Scheduled drugs by the “Pharmaceutical Affairs Law”
– Specified poisonous substances regulated by the “Poisonous and Deleterious Substances Control Law”
– Substances for which manufacturing is prohibited under the “Industrial Safety and Health Law”

5. Usage Procedures

5.1 Submission of Inquiry Form

Please enter proposal details and submit the following inquiry (Google Form) at least six weeks before the experiment date, which is required for discussion with the staff about technical feasibility and schedule availability.

5.2 Preliminary Arrangements

Upon receipt of the inquiry form, JASRI Sample preparation Service staff will contact and discuss preparation details with users. After the discussions, the staff will send user the “Service Confirmation Form (Form PS-B).”

5.3 Submission of the Agreement

Following confirmation the Form PS-B, please provide all information on the “SPring-8 Preparation Service Agreement,” have the person responsible for the payment of fees date and sign the Agreement, and then send it by email to 7.2 Information Desk for Usage Procedure.

5.4 Shipment of Samples

Please make sure that the samples are properly prepared and have been made suitable for each measurement before the shipping. If you have question about preparation of the samples, please contact the staff (See 7.1 Information Desk for Sample preparation Service). Please make sure to send your sample to 7.3 Sample Shipping Address at least two weeks before the experiment date.

Important: To ship the samples from outside Japan, you need to be aware of regulations covering international shipping of chemicals. Please note that you need to go through all steps (e.g. paperwork, customs procedures, etc.) required for entry of the samples to Japan at User’s responsibility and expense.

6. Post-Implementation Processes

The preparation report will be sent to you. After checking the report, please submit the “Notification of Completion of Beamtime” online from the UI site.

Samples will be available at the time of the experiment. For users who did not attend the sessions, the JASRI staff will send back the samples at users’ cost.

The prepared samples obtained through the Sample Preparation Service shall belong to the Organization.

The invoice will be sent to you. Please make sure that your organization makes payment of the fees within 60 days of the invoice date.

7. Contact

7.1 Information Desk for Sample preparation Service

7.2 Information Desk for Usage Procedure

7.3 Sample Shipping Address
　　1-1-1 Kouto, Sayo-cho, Sayo-gun Hyogo 679-5198 JAPAN
　　Japan Synchrotron Radiation Research Institute (JASRI)
　　[Powder diffraction or XAFS] Sample preparation Service (proposal number), SPring-8 Users Office
　　　　e.g. Powder diffraction Sample preparation Service (2022B1234)
　NOTE : For shipping details, please click here.