Aaron Mechler and Chieh Peng

Ampulator

No issues to report.

Balances

A cahn balance set up in the rad van had issues with a dim display. I don't think the issue was found when testing elsewhere. Was moved to storage above coulometer/balance and replaced with another balance.

Carver Presses

No issues to report

Cary Spectrophotometer

• Co-chief Jason Sylvan brought a microplate reader to the ship. He ended up not using it for what he initially planed to use it for. It instead was set up in the chem lab and used to run sulfide, phosphate, and ammonium for comparison to the cary spec.

• This helped reveal an issue with the cary spec as blank values were high; for example, something that should be 0uM phosphate would be read with absorbance of 5-7uM. Initial blanks before a calibration curve were fine but any blanks after would be elevated. Any samples/standards under 15uM were affected with those under 5-10uM having the biggest effect. Over 15uM had no effect or difference. Digging back through past expedition data showed that all post-covid expeditions had concentration baselines of ~4-7uM. Pre-covid expeditions would still obtain down to 0-1uM for samples.

Open

• Looking at the flow cell, there appeared to be a small growth inside it, maybe mold. A new flow cell was installed but the elevated blanks still occurred. The autosampler probe, and all tubing to the flow cell were then replaced. Results were than much better and more accurate for low concentration samples. Bleach was also added to the rinse bottle to help sanitize and clean out sample lines but then returned the rinse bottle to just water. The old flow cell was cleaned with hydrogen peroxide to dissolve and remove the growth.

Coulometer

• Installed a new Coulometer. A spare is in the same place the old spare used to be. The older models are being shipped to shore.

Elemental Analyzer

• Installed a new CHNS. The old CHNS is being shipped to shore. The new CHNS doesn't have a water trap set up so hydrogen peaks are always there. Could install one but it may not need it. Retention times in general were earlier compared to the older CHNS. Can use 600s run times with this new one and still get sulfur.

• Had some problems with nitrogen values when trying to use vanadium pentoxide. Didn't end up using it.

Freeze-dryer

No issues to report.

Fume hoods

No issues to report. Smoke candles were used to test air flow in fume hood. All tested OK

Gas lines/manifold

No issues to report.

GC: NGA1/NGA2/GC2

• Calibrated NGA1 and NGA2.  HS was done previously on 390C so was not done this expedition until U1559D due to seeing what looked like bubbles between the core and liner.

• Used GC2 to run PFT samples. Calibration and running samples went well. Retention times tend to drift over time. Need to adjust calibration retention times every run and check every sample to ensure the peak is being properly identified. Useful to do a calibration with every run.

• During the last batch of samples, a problem was encountered where the autosampler kept bending needles. Looking up troubleshooting help indicated the tension cords in the autosampler need to be changed. After doing that, the autosampler performed normally again. How to change the tension cord, with pictures, was put on the chem lab notebook. It's not a frequent maintenance and I got the impression it's an every 5-10 years type of thing. 

Hydrogen generators

No issues to report

IC

• Troubleshooting issues from the end of 392; the low conductivity on anions was due to a bad detector. Switching the detector to cations also resulted in low baselines of ~370 rather than ~900. The detector will be sent to shore to be repaired. The suppressor peak issue was fixed with new reagents.

• Pressure on anions tended to run a little high at ~8-8.5 but never high enough to cause leaking like with prior high pressure issues. Runs well even with the slightly higher pressure. Near the end of the expedition it was settling at ~8 MPa.

ICP

• Ran ICP on both waters and hard rock samples. 

• Had an issue early on running hard rock where sample occasionally wasn't being aspirated. Narrowed it down to a clog (or leak?) in the autosampler probe and tubing. Everything ran well after replacing the probe.

• Was made aware of differences between ICP and IC data for major elements. Then noticing that these differences started after obtaining the current ICP and were not present on older expeditions with the previous ICP. Could be due to problems with much lower dilutions. Ran the last batch of waters at 250uL to 5 mL, but was still different from the IC. Didn't get around to testing a higher dilution for major elements using the old method dilution which did a 1:100 dilution like the IC. 

Microbiology

• The Koach bench was set up and used to keep a clean area during hard rock sampling.

• A turntable and photo setup was used to take 360 pictures of the hard rock mbio whole rounds.

• "Flame box" was used to clean and scientists used hammer and chisels to break rock pieces in the "flame box"

• The hard shell anaerobic chamber in the cold room was used for sediment processing. We had only one bottle of MBIO mix with only H2. Flushing the chamber with regular MBIO mix with CO2 yield high level of O2 (~1%) inside the chamber. It took about 5 minutes for the catalyst to scrub out O2 to bring level down to 18ppm . N2 bottles were used to flush samples and the airlock for the hard shell anaerobic chamber. The usage rate was higher than normal. We switched the N2 to ship N2 line. We have 2 full N2 bottles and several partial used bottles at end of EXP390. The O2 level never went over 10ppm after a 10 minutes flush for shipboard N2. Soft shell anaerobic chamber was not setup, as both scientists want to process their samples in the cold room

• The freezer in the Cold room failed in the beginning of the expedition. It will be send off at end of 390. One of the 3 incubators in MBIO area was moved into Radvan as both incubators in Radvan did not work. Two new incubators (Fisherbrand Isotemp Undercounter #97990E) are purchased in REQ #2204061JOM. one will replace the freezer in cold room (can be set to -10C) and one will replace the one in MBIO area.

• MB0089 Profiling oxygen microsensor were used for measuring O2 level in sediment cores. All O2 measurement was setup in the DHML lab center countertop

• Hybridization incubator was moved into Radvan, but not used. It will be wipe test and move back the MBIO area

RadVan

• Radvan was heavily used for radioactive S35 tracer (at 10mCi/1mL activity) and isotope 13C, 15N, U-13C, and unlabeled mixture

• A small spill incident happened with S35 as scientist was injecting S35 tracer into a vial containing sediment/media and flushed N2. The vial was slightly over-pressurized. When scientist withdrew the injection needle, small amount tracer sprayed back out onto scientist's left forearm. Although he was wearing a lab coat, small amount of tracer got under the lab coat sleeve. Count off was used generously to wash his forearm. We were able to reduced the amount on his forearm to below Geiger counter limit. All area was cleaned up, wipe tested performed. An incident report was filed to TAMU EHS.

• New method was developed for LSC under 35S-SRR. 

• A proper standard was made by diluting 1uL of S35 tracer into 1000 uL (mL) DIW. Then take 1uL of the 1/1000 dilution standard and mix with 7mL scintillation cocktail. The measured counts (CPM) were then calculated into DPM and total activity.

• Scientist was injecting 10uL into a 5cc sediment and 5 cc media mix.

• The remaining S35 tracer will be kept in the upright incubator (labeled radioactive material) for it to decay. As S35 has half life of 87 days. All liquid and solid rad waste will also be stored in the radvan until post EXP393.

Salinity

no issues to report.

SRA

• Had an issue with the IRCal not connecting. Was due to a loose connection. ETs fixed and rewired that connection so that it wont happen again.

Pipettors

• 2 new pipettors arrived and were given tag numbers.

• Request from ALOs to not just throw pipettors out as they are property in AMS and needed to be decommissioned.

Titrations

Alkalinity

• After being idle for a few weeks, had to recalibrate due to iapso results being off. Couldn't get a good calibration and a small salt deposit was found inside the electrode. After cleaning and rinsing the inside, the calibration was better. Took a very long time to stabilize though.

• From what I can find, this happens over time when stored in KCl as the KCl slowly damages it. Longer storage should be in water. Problem being that after being in water it needs hours of time in KCl to be conditioned before being ready for use. Metrohm has a storage solution that should be good for electrodes for long term storage while also keeping electrodes ready for immediate use.

• Decided to open up a new electrode with the assumption that the solution it's stored in is their storage solution. Calibration and stabilization times were great. The mV values for buffers were shifted from the previous electrode with the result of using a little more acid per titration.

• Put in a req for the electrode storage solution from Metrohm. Want to see if it helps keep these electrodes performing better over time without needing to remember to change the storage solution or changing electrodes.

Chloride

not used.

TOC

• Tried to use. Could not get flow in standby. Everything else seemed to work fine, so I assume it's issues with the frit in the EFC blank preventing gas flow during standby. There's 2 EFC blanks, and neither one seems to work and cleaning the frits hasn't worked. 

• Put in a req for 2 more EFC blanks. 

• Removed the TOC user guides on confluence. There currently is not TOC user guide and what was on confluence was for an older instrument. Apparently no guide has ever been made for the current instrument. Currently have to rely on a blue notebook and notes in the TOC drawer along with the instrument manuals.

Water system

no issues to report

AMI Nitrogen Gas O2 Sensor

• Kept an eye on the O2 level after connecting ship nitrogen to the anaerobic chamber. Saw an increase up to ~10ppm after flushing the chamber.

Misc

• Encountered problems with Agilent software for the ICP and Cary Spec after some IT updates/changes were done. The issue is an error window about an invalid license or missing license and prevents use of the software. Below is the email from Agilent on how to fix it and it'll require MCS help due to needing internet access for the final step.

• Open

  

• Updating manuals in confluence to remove the quick start guides. Many of them were just as long as the user guides or nearly identical; so combining them instead into a single user guide. I think that any new quick start guides should be done as a very brief cheat sheet like what is done for the spec recipe sheet or for the cahn balance weighing. And maybe keeping it as a supplementary item rather than listed as another guide.

• Developed a new protocol to properly dispose of hazardous waste generated in the chemlab. See below

• Properly disposal of chemistry lab hazardous waste

  The following chemical waste are considered hazardous to environment if disposed directly into the ocean or ship drainage system. However, most of these waste can be disposed safely onboard if neutralization and absorbed into solid phase and incinerated.

  Expired epoxy A and B 

  Disposal method – mixed both parts and create solid form. It is safe to dispose the solid form as plastic waste

  Ascarite (CO2 scrubber)

  Disposal method – neutralize with 10% HCl, until pH is close to 7. Liquid can be washed into the chemical drain with lots of water

  Phenol waste (ammonium analysis)

  Disposal method - Phenol can be incinerated into CO2 and water. Absor the waste with chemical absorbent, such as spill kit material or corn cob absorbent. Solid can be incinerated without generating any toxic waste

  Ethanolamine waste (coulometer anode and cathode solution)

  Disposal method – Ethanolamine can be incinerated without generating any toxic waste. Absorb the waste with chemical absorbent, such as spill kit material or corn cob absorbent. Solid can be incinerated without generating any toxic waste.

  HF waste

  Disposal method

  Dry HF related waste such as paper and gloves, separated into plastic and burnable waste. They can be safely incinerated

  HF bottles need to be neutralized with Acid Eater and rinsed with large quantity of water and disposed as cleaned and rinsed plastic bottles.

  Glass tubes (CHNS analysis)

  Disposal method – items can go into broken glass box

  Vermiculite and cat litter do not burn very well. Clay form cat litter actually produce toxic gas when incinerated. A form of absorbent made of corn cob is found and send in in ship REQ390_2. Corncob is biodegradable and incinerable. It can absorb solvent, coolant, oil, and other liquid, but it cannot be used as acid neutralizer.

  Make sure all absorbed material bags are labeled chemistry lab waste, do not open.