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VAC (EYA)
dan.chen - 18:01 Friday 12 April 2024 (29214) Print this report
Pool of liquid in EYA chamber

With Uchiyama, Yokozawa, Yuzu, Takase

We found a pool of liquid the bottom of the EXA like a lake.
The size of the lake was difficult to estimate, but the order is about 1cm in depth and 20cm in diameter.

  • Liquid-like material was seen on the optical table surface, on the Pcal mirrors, and on the H steel.
  • Also there are small drips in the vacuum tube between EYA and EYC.
  • We used a black light to check them, and they looked slightly blue or green.
  • We used a long band and a Kimwipe to get a little of the liquid. To the touch, it was viscous and oily.
  • There was no liquid on the NAB, but there were traces of what appeared to have dried up.

Picture: link

Images attached to this report
Comments to this report:
shinji.miyoki - 8:17 Sunday 14 April 2024 (29220) Print this report

Some members in the KAGRA-PMS mailing lists were called to join the discussion on this topics and discussed where it came from, what is this material, and what should we do for this issue at 23:00 on last Friday.

Anyway, we need more investigation on, such as what is the process, sampling, material identification (in the commercial company), the strategy on how to remove this material, and how to clean it. Kimura-san will check whether he can safely open and close the IFC70 flange at the bottom of this type of vacuum tank on Monday. If possible, we can remove at least the liquid. The cleaning method depends on this liquid material. Uchiyama-kun will also try to reopen the closed IYA tank to check inside. About EXA, the vacuum level is not bad during pumping. So no such material is expected because it should be much worse if it exists.

I just guess the total cleaning of this EYA tank will take ~ one month or so. (Just my guess)

---

The first report some pollution on Tcam mirror in the EYA tank was in February. https://klog.icrr.u-tokyo.ac.jp/osl/?r=28644

hirotaka.yuzurihara - 13:07 Sunday 14 April 2024 (29221) Print this report

>The first report some pollution on Tcam mirror in the EYA tank was in February. https://klog.icrr.u-tokyo.ac.jp/osl/?r=28644

This is just a comment. The dust on the TCam mirror in the EYA tank was cleaned on Friday (klog#29213). The mirror could have been cleaned without a complicated cleaning procedure. So, it seems the dirt on the TCam mirror is caused by something other than the oil-ish liquid in the EYA chamber.

shinji.miyoki - 17:09 Sunday 14 April 2024 (29222) Print this report

One more important investigation was pointed out by Uchiyama-kun at the Friday meeting. That is whether the liquid exists in the cone below or not. We need a flexible fiber scope or some simple inspection tools to check the liquid in the cone below. If it is, the cleaning work can be the reconstruction of the stuff around EYA. Some members are proposing a method to avoid this reconstruction to save time.

tomotada.akutsu - 13:56 Monday 15 April 2024 (29226) Print this report

For your information. My EYA NAB check on Mar 28, 2024 -> 28997

And the attached photos are additional photos from my directory on that day

Images attached to this comment
takafumi.ushiba - 19:02 Monday 15 April 2024 (29230) Print this report

[Akutsu, Ushiba]

We investigated EYA chamber and obtained a sample of the liquid inside the chamber.
We used sysringe with tubes to obtain a sample and stored in the plastic bottole for ethanol.
We also obtained a small amount of the liquid in the stainless bowl.

The  sample volume is about 50 ml and the color of the sample liquid is yellowish (fig1).
Also, I felt the liwuidd is thick during gathering the liquid with syringe.

We stored stainless bowl in the draft chamber to check if the liwuid will be evapolated (fig2, fig3).
We also stored a bottle of the sample at the clean booth of draft chamber (fig4).

Images attached to this comment
tomotada.akutsu - 20:34 Monday 15 April 2024 (29232) Print this report

During this work, we found a white label that has been left in this EYA chamber maybe for 6 years... and detached it.

Images attached to this comment
takafumi.ushiba - 17:03 Tuesday 16 April 2024 (29238) Print this report

[Akutsu, Tamaki, Takano, Ushiba]

First, we checked the viscosity of the liquid yesterday (movie1: sample in the bottle doesn't seem high viscosity. movie2: sample in the bowl seems high viscosity).
Then, we tested if the liquid can be melt in the following things.

1. Water: not melt and liquid is float on the water surface
2. Ethanol: not melt and liquid sank in the ethanol.
3. Aceton: melt easily

We stored all samples in the draft chamber and put labels below each sample.

Non-image files attached to this comment
shinji.miyoki - 21:42 Tuesday 16 April 2024 (29241) Print this report

The speed of melting in the case of acetone is fast or slow or that you need to mix by some bar many times? 

tomotada.akutsu - 21:51 Tuesday 16 April 2024 (29242) Print this report

Additional comment: The difference between the one in bottle and the other in bowl was that the bowl one was left (with its upper opened) in the draft chamber (in operation) for a half day (from yesterday's evening to today's morning) so something might evapolate during this period. The bottle was sealed and was out of the draft chamber.

ryutaro.takahashi - 22:29 Tuesday 16 April 2024 (29243) Print this report

[Ikeda, Takahashi]

We tried to take pictures and movies inside the bottom bellows with the fiber scope. The picture and movie (better quality) show the gap between the pillar and the bellows.

Images attached to this comment
takashi.uchiyama - 17:34 Wednesday 17 April 2024 (29258) Print this report
2024/04/17

Sawada, Kimura, Hayakawa, Uchiyama

We performed several tests on the liquid sample.

[1] PH check
I checked the PH of the sample with a PH checker paper.
The color of the paper showed the PH is between 5 and 6. It means that the liquid has weak acidity.

[2] Pumping down test
We constructed a small vacuum system.
- Firstly, I pumped down the box while the inside was empty. The achieved pressure was 0.2 atm.
- Secondly, I put liquid inside the box and then pumped it down. The achieved pressure was 0.2 atm.
- Finally, I put the liquid added some water in the box, and then pumped it down. The achieved pressure was 0.2 atm.
We can use a strong pumping unit for this test at the next trial.

[3] Burnable test
We put a small amount of liquid in an aluminum bowl and heated it with a lighter.
The liquid was not burned.



takashi.uchiyama - 17:35 Friday 19 April 2024 (29280) Print this report
2024/04/19

Sawada, mTakahashi, Yoshimura, Hayakawa, Uchiyama

We pumped out the liquid in the EYA chamber.
After that, we opened the ICF70 flange at the bottom of the chamber.
We think that most of the liquid was extracted from EYA with these works.

The liquid that was pumped out is kept in a polyethylene tank (10L).
The liquid that was dropped from the ICF70 is kept in a plastic container.
Both the tank and the container are in the draft chamber.

We kept the flange open and put a SUS tray under the flange to catch the liquid.
takashi.uchiyama - 16:27 Tuesday 23 April 2024 (29298) Print this report
2024/04/23

Kimura, Uchiyama

We performed the pumping test again.
This time, we used a stronger dry pomp.

[Trial 1] No sample
The achieved vacuum pressure was 3*10^3Pa.

[Trial 2] with a liquid sample obtained last Friday. https://klog.icrr.u-tokyo.ac.jp/osl/?r=29280
We observed bubbles were generated but finally, the bubble generation stopped.
The achieved vacuum pressure was 3*10^3Pa.

We think that the origin of the bubbles was water.

[Trial 3] with the liquid sample used in the trial 2.
No bubble generation was observed during pumping down.
The achieved vacuum pressure was 3*10^3Pa.

The next time, we will use TMP.



Images attached to this comment
nobuhiro.kimura - 15:37 Thursday 25 April 2024 (29329) Print this report

[Kimura and M. Takahashi]

 To identify the source of the liquid material that entered the EYA tank, three filters of the air compressor and the inside of the connection piping of the dry pumps for vacuum pumping were visually inspected.
As a result of the visual inspection, no traces of liquid material were found inside the filters of the air compressor and the connecting piping of the dry pumps for vacuum pumping.
The smell inside the filter and piping was confirmed by nose, but the same irritating smell observed in the EYA tank was not found.
Three filters of the air compressor were replaced with new ones because more than two years had passed since the last replacement.

takashi.uchiyama - 14:24 Tuesday 30 April 2024 (29359) Print this report
2024/04/30

Uchiyama

I took some photos under the optical table in EYA with a 360-degree camera.

I found that almost all the bottom surfaces of the chamber and the optical table are contaminated.
The support legs of the optical table also are contaminated.
Images attached to this comment
takashi.uchiyama - 9:10 Wednesday 15 May 2024 (29510) Print this report
uchiyama

I evaluated the amount of liquid in EYA.
The result is almost 1L.

I have already provided the liquid to some institutes and a company. The total amount is 220cc.

We are keeping the liquid in several containers.
- Sample in the ethanol bottle: 31.4g ( https://klog.icrr.u-tokyo.ac.jp/osl/?r=29230)
-Sample in polyethylene tank: 585g ( https://klog.icrr.u-tokyo.ac.jp/osl/?r=29280)
-Sample in plastic container:133g( https://klog.icrr.u-tokyo.ac.jp/osl/?r=29280)
The total weight of te liquid in the containers is 749g

If we assume the density of the liquid is 0.9g/cc, The amount of the liquid in the containers is 833cc.

The total amount of the liquid is 1053cc (220cc+833cc).
takashi.uchiyama - 8:41 Thursday 16 May 2024 (29526) Print this report
KEK Environmental Measurement Group

They performed the component analysis of the liquid in EYA.
I uploaded the result report on JGWdoc. The report is written in Japanese.
https://gwdoc.icrr.u-tokyo.ac.jp/cgi-bin/private/DocDB/ShowDocument?docid=15790

They examined a Raman spectrophotometer to the sample liquid and it showed a spectrum similar to the fatty acid ester was obtained.
takashi.uchiyama - 8:59 Thursday 30 May 2024 (29686) Print this report
2024/05/30

We received from the company the results of the component analysis of the EYA liquid.
I uploaded the document at the following JGWdoc link.
https://gwdoc.icrr.u-tokyo.ac.jp/cgi-bin/private/DocDB/ShowDocument?docid=15790

The company performed GC/MS (Gas Chromatography-Mass spectrometry) and FT-IR (Fourier Transform Infrared Spectroscopy).
According to the result of FT-IR, the liquid in EYA was presumed to be triglyceride.
takashi.uchiyama - 15:10 Thursday 30 May 2024 (29695) Print this report
2024/05/30

Uchiyama

The specific gravity of the liquid was measured using a standard specific gravity meter.
The specific gravity of the liquid was 0.947.

This specific gravity is a large value compared to general vegetable edible oils.
takashi.uchiyama - 14:57 Thursday 13 June 2024 (29885) Print this report
2024/06/04

We received the additional component analysis of two kinds of mechanical oil (LVO100, LVO210) used in vacuum pumps of KAGRA.
Spares of those oils are stocked in KAGRA.
The analysis confirmed the liquid EYA is different from the mechanical oils.

The report (chem-A-24-12_修正.pdf) was uploaded in JGWdoc.
https://gwdoc.icrr.u-tokyo.ac.jp/cgi-bin/private/DocDB/ShowDocument?docid=15790
takashi.uchiyama - 14:59 Thursday 13 June 2024 (29886) Print this report
2024/06/07

We received the results of the component analysis from the University of Tokyo. They inspected the liquid in EYA and the mechanical vacuum pump oil (LVO210) stocked in KAGRA.

The results are uploaded in JGWdoc.
https://gwdoc.icrr.u-tokyo.ac.jp/cgi-bin/private/DocDB/ShowDocument?docid=15790

They commented, "As a result, we could not identify the ingredients, but I guess that the high boiling point component jumped from LVO210 and only the low boiling point component remained in this sample."

We should investigate the possibility of whether LVO210 is a liquid in EYA or not.
nobuhiro.kimura - 12:34 Tuesday 25 June 2024 (30099) Print this report

1. Results of Q-mass measurements
 Q-mass measurements of EYC were performed on June 24 and June 25.
The mass detection range is m=2 to m=100.
The displayed values in the attached graphs (Graph 1 ~ 4) refer to two types of total pressure and sensitivity calibration values.
Both graphs show that many partial pressures are distributed between m=16 and m=18.
Since the values are close to the cracking pattern ratios for H2O(m=18) shown below, it is presumed that most partial pressures between m=16 and m=18 are derived from H2O.
Total pressure: 5.44 x 10^-4 Pa
H2O(m=18): 100 % <- 4.1 x10^-4 Pa (100 %)
OH+(m=17): 25 % <- 9.4 x10^-5 Pa (23 %)
O+(m=16): 2 % <- 9.4 x10^-5 Pa (1.4 %)
 The reason for the high EYC pressure is thought to be the result of water deposited on the inner surface of the duct during cleaning inside the EYA and between the EYA and EYC, which continues to be released as outgassing.
 For reference, the partial pressure ratios from m=16 to m=18 before duct shield cooling in December 2022 are shown.
Total pressure: 4.19 x 10^-5 Pa
H2O (m=18): 100 % <- 2.38 x10^-5 Pa (100 %)
OH+(m=17): 25 % <- 5.39 x10^-6 Pa (23 %)
O+(m=16): 2 % <- 4.3 x10^-7 Pa (1.8 %)

2. Vacuum leak estimation
Examine whether a vacuum leak is occurring at EYC.
If the ratio of O2(m=32) to N2(m=28) is 1:4, a vacuum leak may be present.
From the measurement results, the ratio of O2(m=32) to N2(m=28) is
O2(m=32):N2(m=28)=1.19 x10^-6 Pa:3.65x10^-6 Pa=1:3.
In addition, Ar (m=40), which is present in the atmosphere at about 1 %, has a partial pressure (1.25x10^-7 Pa) relative to the total pressure (5.44x10^-4 Pa) in the Q-mass results, which is 0.023 %< 1 %. 
 Based on these results, it is presumed that there is no significant vacuum leakage, but a leak test is necessary to make a final determination.
 
3. About CO2
 CO2 is  estimated to be generated by desorption from the inner surface of a vacuum vessel that is not baking like KAGRA.

Non-image files attached to this comment
nobuhiro.kimura - 18:21 Sunday 21 July 2024 (30496) Print this report

Results of Q-mass measurements
 Q-mass measurements of EYC were performed on July 19 and July 21.
The mass detection range is m=2 to m=100.
The displayed values in the attached graphs (Graph 1 ~4) refer to two types of total pressure and sensitivity calibration values.
Both graphs show that many partial pressures are distributed between m=16 and m=18.
 
On July 19: 
 Total pressure: 1.21 x 10^-4 Pa
 H2O(m=18):  7.0 x10^-5 Pa
 N2 (m=28): 1.2 x 10^-5 Pa
 O2 (m=32): 2.3 x 10^-6 Pa
On July 21: 
 Total pressure: 1.76 x 10^-4 Pa
 H2O(m=18):  5.1 x10^-5 Pa
 N2 (m=28): 2.1 x 10^-5 Pa
 O2 (m=32): 4.8 x 10^-6 Pa
The pressure in the EYC maintains a decreasing trend. The main component of the residual gas is H2O.
The higher pressure on July 21 than that on July 19 is due to the vacuum leak test conducted from July 19 to July 20.

Non-image files attached to this comment
nobuhiro.kimura - 9:00 Tuesday 30 July 2024 (30623) Print this report

Results of Q-mass measurements
 Q-mass measurements of EYC were performed on July 25 and July 30.
The mass detection range is m=2 to m=100.
The displayed values in the attached graphs (Graph 1 ~4) refer to two types of total pressure and sensitivity calibration values.
Both graphs show that many partial pressures are distributed between m=16 and m=18.
 
On July 25: 
 Total pressure: 8.05 x 10^-5 Pa
 H2O(m=18):  5.3 x10^-5 Pa
 N2 (m=28): 2.3 x 10^-6 Pa
 O2 (m=32): 4.0 x 10^-7 Pa
On July 30: 
 Total pressure: 7.24 x 10^-5 Pa
 H2O(m=18):  4.2 x10^-5 Pa
 N2 (m=28): 1.8 x 10^-6 Pa
 O2 (m=32): 4.2 x 10^-7 Pa

Non-image files attached to this comment
takashi.uchiyama - 11:12 Monday 31 March 2025 (33172) Print this report
205/03/31

We received the component analysis of two kinds of mechanical oil (LVO100, LVO210) used in the vacuum pumps in KAGRA.
We pumped out each oil 1400 hours before this analysis. Spares of those oils are stocked in KAGRA.
The analysis confirmed that the liquid EYA is different from the mechanical oils.

The report (chem-A-24-63_LVO100.pdf and chem-A-24-64_LVO210.pdf) was uploaded to JGWdoc.
https://gwdoc.icrr.u-tokyo.ac.jp/cgi-bin/private/DocDB/ShowDocument?docid=15790
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