USAXS Sample Holders for liquid samples
Static samples - Flat sample holders : Grace-Bio Liquid cells
These cells are suitable for water based samples (not containing solvents) at room temperatures. These are single use cells, easy to use and convenient. Please, check gracebio web site:
The cost of these is about $4 per cell (1 sample for JTR13 and JTR20, 8 samples for JTR8R cell), please, buy your own if you plan to use these.
Many users bring Charelss Supper (10 micron walls) capillaries: Capillaries - they are really difficult to use. They break easily and are tough to fill. However, capillaries of more or less any type of glass can be used for USAXS. If you have preferred type, please, use 1.5 mm or 2 mm capillarires, at higher energies even 5 mm capillaries are fine. Thinner capillaries are generally not suitable for USAXS. Since the cost is per capillary is typically subtantial, we cannot provide capillaries to users, please, buy your own and bring them with you.
For users with sufficient amount of sample volume capillaries we tested and succesfully used NMR tubes. The NMR capillaries we have used are 4mm internal diameter, 5mm external diameter, with cap included. They provide ~3x better singal-to-noise ratio than 1mm diameter capillaries if transmisison is reasonable. For water/regular light solvent based samples and 18keV or higher X-ray energies these capillaries work fine. One source of these is here: Fisher scientific Wilmad Thin Walled High Throughput NMR tumeb (cat. No. 16-800-161). We hope to have these at the beamline (100 of these costs ~ $100) but I suggest users buy their own to make sure there is enough fo them. We have currently capillary holder which enables us to measure about 12 at a time as well as heated samples holder (even though temperature homonegeity of these in the heater is not really that good). These capillaries also enable recovery of the sample after measurements. We stock these, but if you plan to use larger amounts of these, please buy your own (or resupply us). The cost is about $1
Alternative capillaries we tested and succesfully used are melting capillaries, much cheaper than dedicated X-ray capillaries and much easier to use - and very good for samples with stronger scattering. One source of these is here: Kimbel Chase KIMAX Melting capillaries. We routinely have these at the beamline (as 100 of these costs ~ $20). Recovery of sample from these is difficult.
Flow cell experiments:
Many users want to use flow cell to measure their liquid samples. This reduces the X-ray damage to the samples and allows users to study changes in the sample as function of time/pH/temperature/... Keep in mind, that filling flow cell is done by hand and is time consuming, Flow cells also need to be cleaned which is not always easy or even possible... We had success with using 4mm internal diameter capillary (the Wilmad NMR tubes) for flow cells and at 21keV they work very well - and they are easy to handle. Users need to provide tubing for their experiments, as it gets contaminated by the samples and needs to be replaced for each user.
Tubing needed to build a flow cell which user needs to provide:
10 feet (3 m) of polytetrafluoroethylene (PTFE) tubing, Source: Fischer Scientific, Part# 0660527 Description: Cole Parmer, Zeus Industrial Products Inc model number 94812, PTFE tubing, 1/16In ID x 1/8In OD, 25 ft/pack
Parts typically provided by beamline, users can procure if they have avaibale funds (check with beamline first)
One foot of thin silicone tubing to connect PTFE tubing to the cell and other connectors, Source: Fischer Scientific, Part# 14179110, Description: Thermo Scientific™ Nalgene™ Pharma-Grade Platinum-Cured Silicone Tubing; 1/8 in (OD), 1/16 in (ID); 50 ft/pack
One foot of thick silicone tubing for the peristaltic pump, Source: Fischer Scientific, Part# 14179114, Description: Thermo Scientific™ Nalgene™ Pharma-Grade Platinum-Cured Silicone Tubing; 3/8 in (OD), 1/4 in (ID); 50 ft/pack
Selected connectors from Cole-Parmer Luer Fitting Kit, Source: Cole-Palmer, Part# EW-45511-00, Description: Cole-Parmer Luer Fitting Kit, Assorted Materials/Sizes, 477 Pieces/Pk
The glass flow cell, cut with a diamond saw from an NMR tube, Source: Fischer Scientific, Part# 16800161, Description: Wilmad™ Thin Walled High Throughput NMR Tubes; ASTM E438 Type 1 Class B glass; 5mm (OD); 0.43mm (wall thickness); 103.5mm (length); 100 pieces
Two small pieces of 3/16 (ID) latex tubing to connect to the glass tube (available at the APS stockroom),