Mail-in/ remote Operation Procedures

Available Sample Holders: 

Instruction on Sample Mounting & Beamline Operation

Register & Request holders

Input Sample Info:

Mail-in/ remote Operation Procedures

Available Sample Holders: 

Instruction on Sample Mounting & Beamline Operation

Register & Request holders

Input Sample Info:

Mail-in/ remote Operation Procedures

Available Sample Holders: 

Instruction on Sample Mounting & Beamline Operation

Register & Request holders

Input Sample Info:

Mail-in/ remote Operation Procedures

Available Sample Holders: 

Request holders

Click to Input Sample Info:

Mail-in/ remote Operation Procedures

Available Sample Holders: 

Request holders

Click to Input Sample Info:

For mail-in and remote operations, a variety of sample holders have been designed and made at 12-ID for room temperature and temperature variation studies. A robot is used at beamline for sample changing. 

(click the above image to watch a video of the robot operation at the beamline)

Below lists the available sample holders and frames.  

1. Holders of Solid and Capillary Samples for Room Temperature Study

A. Holder for Solid SAXS/WAXS Samples

The sample holder shown below is designed for solid samples, including powder, films, etc. Samples can be mounted using tapes. To make the measurements easy, sample size >=2mm is recommended.

Note: Each sample holder may contain many samples. Sample info (sample name, position, x-ray exposure time, etc) is required for remote/mail-in operations. After you obtain the sample holder/frame, use the proper link at side field under "Input Sample Info" to provide sample information. The information is required for all sample holders. 

B. Cartrige for Capillary Samples

The below sample cartrige/holder is designed for capillary samples.  

This cartrige works for both glass/quartz capillaries and kapton capillaries, and can hold capillary up to 3 mm in diameter. Cartridges may be mounted horizontally or vertically in the holder, but not upside-down. Samples are recommended to fill >=20mm. We recommend sealing with Devcon 5 Minute or 2 Ton Epoxy. If you have not used these before, you may need some practice to get a feel for the mixing and hardening times.

Quartz capillary is preferred because of its high mechanic strength. Here are a couple of commerical sources:

•  https://hamptonresearch.com/product-Quartz-Capillaries-325.html  

•  http://www.charles-supper.com/en/page/product.cfm?idProduct=17

Please note:

• The capillary is meant for solution samples, not powders because thick powder sample could saturate detector.

• Solvents with high-Z element (i.e., chloroform) may not work due to high x-ray absorption.

C. Holder for GISAXS/GIWAXS Samples

The below holder is for GISAXS/GIWAXS samples. Chips samples can be mounted using double side tapes.

 

D. Ambient DSC Pan Holder

Below is the sample holder of DSC pans. It is designed for the standard TA instruments aluminum Hermetic pans (TA instruments cat.#: 900793.901(pans) and 900794.901(lids), or pans with same dimensions.

Universal frame for sample holders A-D and Robotic Operation

A universal frame is designed to hold sample holders A-D.  Below shows the assembles of sample holders and frames. Left: the model of an assemble of a capillary cartrige/holder (in yellow color) and a frame (in cyan color). Right: a picture of an assemble of a solid sample holder and a frame, both being 3-D printed.

Each frame has a unique ID#, matching the sample holder type.  A magnetic mount is attached at the bottom of the frame, for the sample mounting at the beamline. Sample change is performed by a robotic arm at the beamline. 

Note:  (1) When a sample holder is requested, a frame will be sent with the sample holder.

             (2) At the beamline, the "Source Side" will face the X-ray source, and the sample numbering is based on the "Source side" as below.

2. Holders of Solid and Capillary Samples for Temperature Variation Study

Remote temperature study is also available at 12-ID, using the home-made sample heater shown below. The temperature range covers from 20 - ~350C.

Available sample holders list blow.

E. Temperature Capillary Holder

Below is the model of temperature capillary holder, for standard capillaries listed in B.

F. Temperature DSC Holder

Below is the model of temperature DSC pan holder, for standard DSC pans listed in D.

 

3. Mail-in / Remote Operation for Bio and Other Liqud Samples (Non-Capillary) 

G. BioSAXS and other Aqueous Samples

We use both 0.5ml tubes and 96-well plates for Bio or other aqueous samples. 

0.5ml tubes are only used for mail-in services. Samples should be well labeled either on the cap or the side of the 0.5ml tubes, volume >=140 uL, and ready to go after centrifugation. If labeled on the size/body of the tubes, use permenant marker only, no tapes, otherwise, the the tubes will be too fat to fit in the sample holder.

Provide sufficient buffer solution, both in 0.5ml tubes (for measurements) and large tube (for flow cell washing).   
Recommended 0.5ml tube:  https://us.vwr.com/store/product/4674090/vwr-slick-disposable-microcentrifuge-tubes-polypropylene

96-well plates can be used for both mail-in and remote operations.

The beamline autosampler uses Thermo Scientific non-skirted 96-well PCR plates (Cat#: AB-0600B, and Dimensions & Model) or 96-well plates from other sources but with same dimensions. The well holds up to 0.3 mL.

Note: Users should buy their own 96-well plates. However, users are still asked to register and "request" plates for mail-in and remote operation. After receiving the requests, instead of sending 96-well plates, beamline staff will email web links for recording sample information, which will be used in experiments.

The 96-well plates should be sealed with pierceable aluminum sealing films. Below is one example from Sigma. Instruction on preparing and packing 96-well plates can be found here: 96-well plate preparation and packing. 

               
   

The 0.5ml tubes and 96-well plates can be run using a home-made autosampler as shown below.

       
autosampler running 0.5 ml tubes.                                     autosampler running 96-well plate

H. Non-bio Liquid Samples

2ml glass vials (blow, left) with septa are used for non-bio or organic liquid samples. The sample holder(below, right) can hold up to 60 vials.

The specification of vial: diameter 12mm, height 32mm, top cap open 9mm, hole 6mm.

Commerical source of the vial: https://www.fishersci.com/shop/products/fisherbrand-vials-closures/13622186