Report on HD gas analysis by Raman spectroscopy...

Summary Report on HD gas analysis by Raman spectroscopy technique - June - September - November 2015.Check measurements – November 2016

- Introduction.Seven bottles of HD gas were sent to Rome from JLab. They were received May 2015.The seven bottles contained HD gas as follows:1. JMU 6.1 tank #6 filled 1/21/152. JMU 5.1 tank #1 filled 1/22/153. JMU 6.1 tank #19 filled 1/23/154. JMU 6.1 tank #31 filled 2/4/155. JMU 6.1 tank #4 filled 2/5/156. JMU 6.0 uva tank #9 filled 2/7/157. JMU 2 reference tank filled 1/15/2013

The Laser was serviced early 2015; the final power available on the green line was 12 W. The power slowly reduced to 9W. The average counting rate available at the highest HD peaks was typically higher than 2000 counts/s. More data were taken one year later in October 2016 with a Laser power of 8W. The power is down at 6W in March 2017.

We took a first set of measurements on June 6-8 2015 and July 14-20 2015. A second set of measurements was taken from September 15th to September 17th for double check. A third set of measurements was taken on November 19-25 2015. Each spectrum is analyzed in two different methods to extract the peaks content (using either the integral under the Gaussian function or the sum of histogram counts after the background subtraction): we have a total of 4 quasi-independent determinations of the relative gas concentrations.

The analysis program was revised to better take into account the noise level and the final error was evaluated taking into account the correlation among the results (following g14 data analysis 2 based procedure). All the 2015 data have been re-analyzed and were the subject of Martina Laurenza undergraduate thesis.

To better understand the results a final set of data has been take on October 19-21 2016.

1. JMU6.1 tank # 6 Measurements list: June 8th high noise at high wave-lenghts (neon on?) September 15th some air is present November 25th air is still present October 19th 2016 some air present – high recombination

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a. 15/6/8 JMU-6.1 tank#6 HD gas was used to fill the Raman cell and we took a Raman spectrum on June 8th 2015 lasting 1 hour. The maximum count rate on the highest peak was increased to more than 2000 counts/s.

jmu6-1 tank 6 15_6_8 - neon - 2434 max counts method H2/HD Δ (H2/HD) D2/HD Δ(D2/HD)fit-ga+b 0,00065 0,00002 0,00062 0,00004ref-ga+b 0,00068 0,00003 0,00066 0,00007fit-int-back 0,00068 0,00003 0,00065 0,00005ref-int-back 0,00068 0,00003 0,00066 0,00007

mean 0,00066 0,00002 0,00064 0,00003

Figure 1. JMU6-1 tank 6 Raman analysis results of June 8th a) spectrum b) analysis results. Both H2 and D2 lines are at the low.

Figure 1 shows the spectrum and the Table of results from the 4 quasi-independent analyses. H2 and D2 concentrations are very similar. The final results are:

H2/HD = ( 0,000660,00002)D2/HD = ( 0,000640,00003)

b. 15/9/15 The cell was filled and measured again for 1 hour on September 15 th. Some air is present in the cell but it does not prevent to extract the D2 content of the first peak.

jmu6-1 tank 6 15_9_15 - air - 1194 max counts method H2/HD Δ (H2/HD) D2/HD Δ(D2/HD)fit-ga+b 0,00093 0,00005 0,00107 0,00009ref-ga+b 0,00096 0,00006 0,00080 0,00010fit-int-back 0,00093 0,00006 0,00110 0,00010ref-int-back 0,00095 0,00006 0,00080 0,00010

mean 0,00094 0,00006 0,00095 0,00008

Figure 2. JMU6-1 tank 6 Raman analysis results of September 15th a) spectrum b) analysis results. H2 and D2

concentrations are higher than in June.

Figure 2 shows the spectrum and the Table of results. H2 and D2 concentrations increased. The final results are:

H2/HD = ( 0,000960,00006)D2/HD = ( 0,000950,00008)

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c. 15/11/25 The cell was filled and measured again for 1 hour on November 18th. Some air is still present in the cell.


mean 0,00201 0,00008 0,00191 0,00008

Figure 3. JMU6-1 tank 6 Raman analysis results of November 25 th a) spectrum b) analysis results. H2 and D2

concentrations keep incresing.


H2/HD = ( 0,002010,00008)D2/HD = ( 0,001910,00008)

d. 16/10/19 The cell was filled and measured again for 1 hour on October 19th 2016. Some air is still present in the cell.

Figure 4. JMU6-1 tank 6 Raman analysis results of October 19th a) spectrum b) analysis results. H2 and D2

concentrations are one order of magnitude higher.


H2/HD = ( 0,023000,00020)D2/HD = (0,024000,00030)

2. JMU6.1 tank # 1

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mean 0,02300 0,00020 0,02500 0,00030

Measurements list: June 9th some air is present September 15th good spectrum November 19th good spectrum

a. 15/6/9 JMU-6.1 tank#1 HD gas was used to fill the Raman cell. The spectrum contained some air and lasted one hour. Both H2 and D2 gas are present at the same level of 1x10 -3. The maximum counts is again higher than 2000 counts/s

jmu6-1 tank 1 15_6_9 - 2250 max counts method H2/HD Δ (H2/HD) D2/HD Δ(D2/HD)fit-ga+b 0,00106 0,00003 0,00111 0,00005ref-ga+b 0,00108 0,00003 0,00112 0,00008fit-int-back 0,00106 0,00003 0,00111 0,00006ref-int-back 0,00107 0,00003 0,00110 0,00008

mean 0,00107 0,00003 0,00111 0,00006

Figure 5. JMU6.1 tank 1 Raman analysis results of June 19 th a) spectrum b) analysis results. H2 and D2

concentrations are the same, in the 1x10-3 range.

Figure 5 shows the spectrum and the Table of results. The final results are:H2/HD = ( 0,001070,00002) D2/HD = ( 0,001110,00006).

b. 15/9/15 JMU-6.1 tank#1 HD gas was used to refill the Raman cell and to take a second spectrum for one hour. The spectrum contains no air and has a nice shaped background. Both H2 and D2 gas are present at the same level of 1.4x10-3. Recombination occurred!


mean 0,00143 0,00005 0,00135 0,00005

Figure 6. JMU6.1 tank 1 Raman analysis results of September 15 th a) spectrum b) analysis results. H2 and D2

concentrations are the same, in the 1.4x10-3 range.

Figure 6 shows the spectrum and the Table of results. The final results are:H2/HD = ( 0,001430,00005)

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D2/HD = ( 0,001350,00005).

c. 15/11/19 JMU-6.1 tank#1 HD gas was used to refill the Raman cell and to take a third spectrum for one hour. The spectrum contains no air and has a nice shaped background. Both H2 and D2 gas are present at slightly different levels. Recombination is still evident.


mean 0,00188 0,00005 0,00145 0,00005

Figure 7. JMU6.1 tank 1 Raman analysis results of November 19th a) spectrum b) analysis results. H2 and D2

concentrations are slightly different, in the 1.5x10-3 range.Figure 7 shows the spectrum and the Table of results. The final results are:

H2/HD = ( 0,001880,00005) D2/HD = ( 0,001450,00005).

3. JMU6.1 tank # 19 Measurements list: June 10th some air is present September 16th air present November 19th air present October 20th 2016

a. 15/6/10 JMU-6.1 tank#19 HD gas was used to fill the Raman cell on June 10 th. Gas is contaminated by air. There is lower D2 content at the level of 8 10-4. H2 is slightly higher.


mean 0,00127 0,00002 0,00085 0,00004

Figure 8. JMU6.1 tank #19 Raman analysis results of June 10th a) spectrum b) analysis results. Air contamination is present. D2 concentrations is in the 8 10-4 range, lower than H2.

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Figure 8 shows the spectrum and the Table of results. Air is visible. The final results are:

H2/HD = (0,00127 0,00002) D2/HD = (0,00085 0,00004).

b. 15/9/16 JMU-6.1 tank#19 HD gas was measured again on September 16th. Gas is still contaminated by air. Results are compatible with the first measurement


mean 0,00139 0,00002 0,00086 0,00004

Figure 9. JMU6.1 tank #19 Raman analysis results of September 16th a) spectrum b) analysis results. Air contamination is present. H2 and D2 and concentrations are slightly higher than previous measurement.


H2/HD = ( 0,001390,00002) D2/HD = ( 0,000860,00004).

c. 15/11/19 JMU-6.1 tank#19 HD gas was measured again on November 19 th. Gas is still contaminated by air. H2 concentrations slightly increase while D2 do not.


mean 0,00159 0,00005 0,00085 0,00005

Figure 10. JMU6.1 tank #19 Raman analysis results of November 19 th a) spectrum b) analysis results. Air contamination is present. H2 is slightly higher than previous measurement, D2 is not.

Figure 10 shows the spectrum and the Table of results. Air is visible.

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The final results are:H2/HD = ( 0,001590,00005) D2/HD = ( 0,000850,00005).

d. 16/10/20 JMU-6.1 tank#19 HD gas was measured again on October 20th 2016. Air contaminated is very small. H2 concentrations slightly increase while D2 do not.


mean 0,00175 0,00006 0,00075 0,00005

Figure 11. JMU6.1 tank #19 Raman analysis results of October 20 th a) spectrum b) analysis results. Air contamination is present. H2 is slightly higher than previous measurement, D2 is not.


H2/HD = ( 0,001750,00006) D2/HD = ( 0,000750,00005).

4. JMU6.1 tank # 31 Measurements list:July 14th contains air September 16th contains airNovember 19th contains airOctober 21th 2106 contains air

a. 15/7/14 JMU-6.1 tank#31 HD gas was used to fill the Raman cell on July 14 th. Gas is contaminated by air. D2 is at the 4x10-4 level, H2 content is three times higher respect to D2

content.

jmu6-1 tank 31 15_7_14 - 1884 max counts method H2/HD Δ (H2/HD) D2/HD Δ(D2/HD)fit-ga+b 0,00165 0,00004 0,00042 0,00005ref-ga+b 0,00167 0,00004 0,00034 0,00009

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fit-int-back 0,00166 0,00004 0,00042 0,00006ref-int-back 0,00166 0,00004 0,00034 0,00009

mean 0,00166 0,00004 0,00040 0,00005

Figure 12. JMU6.1 tank #31 Raman analysis results of July 14th a) spectrum b) analysis results. Air contamination is present. H2 concentrations are four times D2 concentrations.


H2/HD = (0,00166 0,00004) D2/HD = (0,00040 0,00005).

b. 15/9/16 JMU-6.1 tank#31 HD gas was measured again on September 16th. Gas is not contaminated by air. Does match previous measurement with a slight increase of concentrations.

Figure 13. JMU6.1 tank #31 Raman analysis results of September 16 th a) spectrum b) analysis results. Air contamination is present. Results are compatible, H2 contamination is slightly higher than in previous measurements.

Figure 13 shows the spectrum and the Table of results. The final results are:

H2/HD = ( 0,001690,00003)

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mean 0,00169 0,00003 0,00041 0,00003

D2/HD = ( 0,000410,00003).

c. 15/11/19 JMU-6.1 tank#31 HD gas was measured again on November 19th. Gas is not contaminated by air. High recombination occurred.

Figure 14. JMU6.1 tank #31 Raman analysis results of November 19 th a) spectrum b) analysis results. Air contamination is present. Huge recombination occurred.

Figure 14 shows the spectrum and the Table of results. Huge recombination is observed.The final results are:

H2/HD = ( 0,043500,00030) D2/HD = ( 0,046600,00020).

d. 16/10/21 JMU-6.1 tank#31 HD gas was measured again on October 21 th 2016. Gas is not contaminated by air. Does match the second measurement with a slight increase of concentrations.

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mean 0,04350 0,00030 0,04660 0,00020


mean 0,00270 0,00030 0,00400 0,00040

Figure 15. JMU6.1 tank #31 Raman analysis results of October 21 th 2016 a) spectrum b) analysis results. Lower recombination is observed.

Figure 15 shows the spectrum and the Table of results. Much lower recombination is observed.The final results are:

H2/HD = ( 0,002700,00030) D2/HD = ( 0,004000,00040).

5. JMU6.1 tank # 4 Measurements list: July 15th no air – neon? September 16th some air is present November 20th no air is present

a. 15/7/15 JMU-6.1 tank#4 HD gas was used to fill the Raman cell on July 15 th. H2 is in the low 10-3 and D2 in the high 10-4 level.

jmu6-1 tank 4 15_7_15 - 1611 max count method H2/HD Δ (H2/HD) D2/HD Δ(D2/HD)fit-ga+b 0,00113 0,00004 0,00078 0,00007ref-ga+b 0,00115 0,00004 0,00080 0,00010fit-int-back 0,00113 0,00009 0,00080 0,00010ref-int-back 0,00114 0,00005 0,00080 0,00010

mean 0,00114 0,00004 0,00079 0,00009

Figure 16. JMU6.1 tank 4 Raman analysis results of July 15 th a) spectrum b) analysis results. H2

concentrations are higher than D2 concentrations in the low 10-3 range.


H2/HD = (0,00114 0,00004) D2/HD = (0,00079 0,00009).

b. 15/9/16 JMU-6.1 tank#4 HD gas was used to fill the Raman cell on September 16th. H2 and D2 content slightly increased compared with previous measurement.

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mean 0,00134 0,00004 0,00102 0,00003

Figure 17. JMU6.1 tank 4 Raman analysis results of September 16 th a) spectrum b) analysis results. H2

concentrations and D2 concentrations are in the low 10-3 range. Figure 17 shows the spectrum and the Table of results. The final results are:

H2/HD = (0,00134 0,00004) D2/HD = (0,00102 0,00003).

c. 15/11/20 JMU-6.1 tank#4 HD gas was used to fill the Raman cell again on November 20 th. H2 and D2 content higly increased compared with previous measurements.


mean 0,05390 0,00010 0,06020 0,00020

Figure 18. JMU6.1 tank 4 Raman analysis results of November 20th a) spectrum b) analysis results. H2

concentrations and D2 concentrations are highly increased.


H2/HD = (0,05390 0,00010) D2/HD = (0,06020 0,00020).

d. 16/10/20 JMU-6.1 tank#4 HD gas was used to fill the Raman cell again on October 20 th

2016. H2 and D2 contents are reduced compared with previous measurements.

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Figure 19. JMU6.1 tank 4 Raman analysis results of October 20th a) spectrum b) analysis results. H2

concentrations and D2 concentrations are reduced.


H2/HD = (0,00235 0,00050) D2/HD = (0,00198 0,00100).

6. JMU6.0 uva tank # 9 Measurements list: July 15th no air September 17th some air November 20th no air

October 21st 2016a. 15/7/15 JMU-6.0 uva tank#9 HD gas was used to fill the Raman cell on July 15 th. H2 and D2 contents are similar, in the mid 10-3 level.

jmu6-0 uva tank 9 15_7_15 - 1689 max counts method H2/HD Δ (H2/HD) D2/HD Δ(D2/HD)fit-ga+b 0,00686 0,00004 0,00623 0,00007ref-ga+b 0,00690 0,00004 0,00640 0,00010fit-int-back 0,00690 0,00004 0,00630 0,00020ref-int-back 0,00690 0,00006 0,00640 0,00010

mean 0,00689 0,00004 0,00631 0,00005

Figure 20. JMU6.0 uva tank 9 Raman analysis results of July 15 th a) spectrum b) analysis results. H2 and D2

concentrations are similar, in the mid 10-3 range. Figure 20 shows the spectrum and the Table of results.

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mean 0,00235 0,00050 0,00198 0,00100

The final results are:H2/HD = (0,00689 0,00004) D2/HD = (0,00631 0,00005).

b. 15/9/17 JMU-6.0 uva tank#9 HD gas was used to fill the Raman cell on September 17th. H2 and D2 are in the in the high 10-4 level.


mean 0,00923 0,00005 0,00897 0,00005

Figure 21 JMU6.0 uva tank 9 Raman analysis results of September 17 th a) spectrum b) analysis results. H2

and D2 concentrations are in the high 10-3 range and increased respect to the previous measurement.Figure 21 shows the spectrum and the Table of results. The final results are:

H2/HD = (0,00923 0,00005) D2/HD = (0,00897 0,00005).

c. 15/11/20 JMU-6.0 uva tank#9 HD gas was used to fill the Raman cell on November 20th. H2 and D2 show high recombination


mean 0,05520 0,00010 0,06110 0,00010

Figure 22 JMU6.0 uva tank 9 Raman analysis results of November 20 th a) spectrum b) analysis results. H2

and D2 concentrations are in the 10-2 range and highly increased respect to the previous measurement.


H2/HD = (0,05520 0,00010) D2/HD = (0,06110 0,00010).

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d. 16/10/21 JMU-6.0 uva tank#9 HD gas was used to fill the Raman cell on October 21th2016. H2 and D2 show high recombination


mean 0,02010 0,00070 0,01900 0,00060

Figure 23 JMU6.0 uva tank 9 Raman analysis results of October 21 th a) spectrum b) analysis results. H2 and D2 concentrations are in the 10-2 range but reduced with respect to the previous measurement.


H2/HD = (0,02010 0,00070) D2/HD = (0,01900 0,00060).

7. JMU2 - reference Measurements list: July 20th air is present September 17th no air November 25th air is present October

a. 15/7/20 JMU-2 reference HD gas was used to fill the Raman cell on July 20th. H2 and D2

contents are comparable, in the mid 10-3.

jmu2 ref 2015 15_7_20 - 2007 max counts method H2/HD Δ (H2/HD) D2/HD Δ(D2/HD)fit-ga+b 0,00505 0,00004 0,00579 0,00006ref-ga+b 0,00506 0,00004 0,00588 0,00009fit-int-back 0,00510 0,00006 0,00588 0,00010ref-int-back 0,00505 0,00005 0,00590 0,00010

mean 0,00506 0,00004 0,00584 0,00006

Figure 24. JMU2 ref Raman analysis results of July 20 th a) spectrum b) analysis results. H2 and D2

concentrations in the mid 10-3 range.

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H2/HD = (0,00506 0,00004) D2/HD = (0,00584 0,00006).

b. 15/9/17 JMU-2 reference HD gas was used to fill the Raman cell on September 17 th. H2 and D2 are in the in the high 10-3 level.


mean 0,00521 0,00003 0,00572 0,00004

Figure 25 JMU6.1.10 SS tank 5 Raman analysis results of September 19 th a) spectrum b) analysis results. H2

and D2 concentrations are in the high 10-3 range. Figure 25 shows the spectrum and the Table of results. The final results are:

H2/HD = (0,00521 0,00003) D2/HD = (0,00572 0,00004).

c. 15/11/25 JMU-2 reference HD gas was used to fill the Raman cell on November 25 th. H2 and D2 are in the in the high 10-3 level.


mean 0,00636 0,00003 0,00729 0,00005

Figure 26 JMU6.1.10 SS tank 5 Raman analysis results of November 25 th a) spectrum b) analysis results. H2

and D2 concentrations are in the high 10-3 range. Slightly increased.Figure 26 shows the spectrum and the Table of results. The final results are:

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H2/HD = (0,00636 0,00003) D2/HD = (0,00729 0,00005).

d. 15/11/25 JMU-2 reference HD gas was used to fill the Raman cell on March 23rd 2017. H2 and D2 are in the in the high 10-3 level.

jmu2 ref 2017_03_23 - 29 max counts method H2/HD Δ (H2/HD) D2/HD Δ(D2/HD)fit-ga+b 0,03097 0,00200 0,00609 0,00200ref-ga+b 0,03450 0,00200 0,00614 0,00200fit-int-back 0,02380 0,01000 0,00690 0,01000ref-int-back 0,03180 0,00200 0,00591 0,00080

mean 0,03027 0,00100 0,00600 0,00070

Figure 27 JMU6.1.10 SS tank 5 Raman analysis results of November 25 th a) spectrum b) analysis results. H2

and D2 concentrations are in the high 10-4 range. Slightly increased.Figure 27 shows the spectrum and the Table of results. The final results are:

H2/HD = (0,03027 0,00100) D2/HD = (0,00600 0,00070).

2. Final measured data table

H2/HD Gas June-July September 15-17 November 18-25 October 17-21 2016 FinalJMU 6.1 tank #6 0,00067 0,00002 0,00095 0,00005 0,00200 0,00003 0,02300 0,00020

JMU 6.1 tank #1 0,00107 0,00003 0,00143 0,00005 0,00188 0,00005

JMU 6.1 tank #19 0,00122 0,00002 0,00139 0,00002 0,00159 0,00005 0,00175 0,00006

JMU 6.1 tank #31 0,00166 0,00004 0,00169 0,00003 0,04349 0,00030 0,00270 0,00030

JMU 6.1 tank #4 0,00114 0,00004 0,00134 0,00004 0,05390 0,00010 0,00235 0,00100

JMU 6.0 UVa #9 0,00689 0,00004 0,00923 0,00005 0,05520 0,00010 0,02007 0,00070

JMU 2 reference 0,00506 0,00004 0,00521 0,00003 0,00636 0,00004 0,03231 0,00140

D2/HD Gas June-July September 15-17 November 18-25 October 17-21 2016 FinalJMU 6.1 tank #6 0,00064 0,00004 0,00099 0,00008 0,00190 0,00010 0,02500 0,00030

JMU 6.1 tank #1 0,00111 0,00006 0,00135 0,00005 0,00145 0,00005

JMU 6.1 tank #19 0,00085 0,00004 0,00086 0,00004 0,00085 0,00005 0,00075 0,00005

JMU 6.1 tank #31 0,00040 0,00005 0,00051 0,00009 0,04660 0,00030 0,00405 0,00040

JMU 6.1 tank #4 0,00079 0,00009 0,00102 0,00003 0,06020 0,00020 0,00198 0,00100

JMU 6.0 UVa #9 0,00631 0,00005 0,00897 0,00005 0,06110 0,00010 0,01900 0,00060

JMU 2 reference 0,00584 0,00004 0,00572 0,00006 0,00729 0,00008 0,00600 0,00070

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