I had this issue with our old CM-10 for either of two reasons: either somehow the temperature sensor on the side on the ODP was out of position, or the cooling water line was clogged, and didn’t have suffi cient fl ow. T e sensor got jogged out of position once during maintenance so that it wasn’t making proper contact with the pump and read wrong. T is shut down the diff usion pump. T e clogged cooling line was commonplace and easily fi xed by running a bottle of CLR (Calcium Lime Rust), a US brand of scale remover, through the lines. T e line could also be cleaned with a liter of 3% H 2 O 2 or 100 mL of 30% H 2 O 2 . In our case, the TEM was on a Haskris chiller, so I just added the solution to the chiller’s water tank and let the cooling water circulate for 4 hours - overnight (depending on how bad things were), then several changes of water until crud quit coming out of the cooling line. If you’re on city water and not a cooler, try removing the in-line fi lter from the housing and adding the H 2 O 2 to the fi lter housing. T is worked on an old ISI EM — except at that lab, we had a problem with biofi lm, not corrosion, and used bleach. Note: the cooling water coming in gets split into two lines in the CM-10, one to the ODP and one to the electronics. If there is a line clog at or aſt er the split, the pump can overheat without aff ecting the electronics, and vice-versa. Phil Oshel Tue Dec 5 It could be the sensor itself problem, but mostly it can come from

the water fl ow or too low of pressure. You need to get the necessary fl ow rate. Michel Ribardière Sun Dec 10 Is there adequate water fl ow in the DP site glass? Are the tops of the cooling coils on the DP cool to the touch? Occasionally the reducer in the water line gets clogged with debris. Mike Calabrese michael. Sun Dec 10

SEM: inert sample transfer

I would like to get some advice/input from folks that have worked with air sensitive and moisture sensitive samples for SEM-EDS. What are some of the methods and best practices to get the sample from the glovebox into the SEM without exposing, and thus modifying, the sample? T anks in advance! David Reuschle Sun Dec 10

We do some work with Li-ion batteries. I built an airlock chamber for our SEM that I would purge with N 2 or Ar, and then we used the South Bay Technologies Sample Savers to transfer the specimen from the glove box to the airlock chamber on the SEM. It was adequate. Brad Johnson Mon Dec 11

Quantomix capsules from the EM suppliers might work. You can seal them in the glovebox and easily transport them to the SEM. Rich Hailstone Mon Dec 11

I have designed specimen rods that protect specimens from air during transfer between a glove box and the microscope. If I can be of help, let me know. Wil Bigelow Sun Dec 10 I would be interested in hearing or seeing more about some of these designs. We had a chamber built for our JEOL 840A that mated with its load-lock. T ere was always some question about the atmosphere in the load-lock that we were exposing the sample to during pump-down. It certainly limited exposure to air. T ere are at least two commercial products that might be suitable. I have no vested interest in them. pp3004-quicklok-ambient-temperature-airlock transfer-module.html

Currently, we are running a Quant 250. We do not have a means to positively control the opening or a door or hatch. We made a small


chamber with a swing-away door on the top. We load the chamber and close the door in a glove box and pump down the chamber. We mount the chamber in the SEM, and a torsion spring swings the door open when chamber pressure gets low enough in the SEM. It does pretty well and would do even better if we could guarantee that the SEM was pumping down from an inert atmosphere. Warren Straszheim Mon Dec 11

SEM: fi laments burn out immediately Our SEM JSM5600LV burns fi laments immediately upon turning high tension ON. T ere was a thunderstorm here, and aſt er a big thunder, the microscope went completely OFF while there was no power cut. Very soon the microscope’s power came back and worked normally, but I noticed the image was bit noisy and defi nition less high. T en I switched it off overnight, and today I started and realized the problem (aſt er I burned a couple of fi laments). Any comment or suggestion will be greatly appreciated. Yorgos Nikas Fri Nov 17 T anks to everybody provided ideas about the problem. We found a faulty voltage regulator in the HT I/O board. T is regulator provides a 39V power rail to the HT Drive board, used by the fi lament current generating circuit. T e regulator had failed, resulting in an overvoltage of some 70V going to the fi lament circuitry, probably causing more damage there (we replaced the regulator, but it was destroyed instantly). Finally, we replaced the faulty voltage regulator, the HT drive board and the HV power supply in the oil tank. I was lucky to have spares for the last two. T e microscope now works fi ne. T e only thing that we still try to solve is that the readings on the SEM menu regarding gun alignment values seem to be incorrect. Also, when we turn HT on, the value of the current fl uctuates for several seconds before stabilizing to the expected value. Since the HT board and power supply are coming from another microscope, it may need some sort of reset that we haven’t found yet. Has anybody any clue? Yorgos Nikas Wed Nov 29

SEM-CL: missing red wavelengths

Does anybody know why an SEM-CL instrument could be missing the red-to-orange wavelengths of the cathodoluminescence spectrum? I run a JEOL 6010LA benchtop SEM with a recently acquired Gatan MonoCL4 cathodoluminescence spectrometer. It works great for zircons, quartz, etc., but picks up little to no signal in the red to orange part of the spectrum even on samples that glow brilliant red under our ancient optical cold-cathode Luminoscope. I checked the same samples out on a ChromaCL hooked up to a Hitachi S3400 in another lab, and there is a similar lack of red signal. I’ve checked, and the accelerating voltages on the Luminoscope are about the same as on the SEM, although the Luminoscope has higher beam current, so I’m not sure why the SEM-CL instruments doesn’t pick up the red luminescence. I’ve read that fi lters placed in front of a detector can eliminate red-orange luminescence and phosphorescence (Reed and Milliken, Journal of Sedimentary Research 73.2: 328-332). T ere was no mention of such a fi lter in the Gatan datasheets for either the ChromaCL or the MonoCL4, but that seems to me to be one possible explanation for the lack of red lumines- cence in SEM-CL compared to optical cold-cathode CL. I’ve leſt a message with Gatan but haven’t heard back yet. Has anybody else with SEM-CL encountered a similar problem, or know of any fi xes? We got the MonoCL4 partly to look at carbonate cements in rocks, so it’s pretty important that we fi gure out how to get good spectra and images in the red and orange zones. Any help would be appreciated. Isabel Barton Fri Nov 17 • 2018 March

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