実験報告書様式（CROSS 開発課題）
承認日 Date of Approval 2014/08/21
承認者 Approver Kaoru Shibata
提出日 Date of report 2014/8/21

Experimental Report
実験課題番号 Project No.

装置責任者 Name of Instrument scientist

2013I0102

Kaoru Shibata

実験課題名 Title of experiment

装置名 Name of Instrument/（BL No.）

Development of sample environmental equipment including highDNA / BL02

pressure and gas atmosphere introduction

利用期間 Dates of experiments

実験責任者名 Name of principal investigator

2013/04/09 09:00 ~ 2013/04/12 07:00

Takeshi Yamada

2014/03/27 21:00 ~ 2014/03/30 21:00

所属 Affiliation

2014/03/21 09:00 ~ 2014/03/22 09:00

CROSS-Tokai
１．研究成果概要（試料の名称、組成、物理的・化学的性状を明記するとともに、実験方法、利用の結果得られた主なデータ、考察、結論、図表等を記述してください。
Outline of experimental results (experimental method and results should be reported including sample
information such as composition, physical and/or chemical characteristics.
The aim of this CROSS Development Project is to perform the development and to do test
experiments for the following two type sample environment equipment as taking advantage of thecharacteristics of high energy resolution spectrometer DNA (BL02).
(A). An in situ water vapor and gas atmosphere introduction equipment(B). A high-pressure generation equipment (P< 2000 atm)
In 2013 period, the water vapor introduction experiments with the gas introduction equipment wereperformed as described below. The high-pressure generation equipment was prepared in the 2013 year
CROSS budget. However, time of the pre-test is not enough thus, the beam experiment was not
performed in 2013. This will be performed in 2014.
The water vapor introduction experiments on Nafion® membrane were performed by using the gas
atmosphere introduction equipment mounted on the BL02 top-loading cryostat and using BL02
spectrometer with 13 µeV energy resolution. The schematic image of the gas atmosphere introduction
system is shown in Fig. 1. The vapor pressure was controlled by the auto control pressure regulated
valve (valve P on Fig. 1).

Fig. 1. Schematic image of the gas
atmosphere introduction system.

Fig. 2. Plots of elastic intensity and setting
relative pressure of the water vapor.

１．研究成果概要（つづき） Outline of experimental results (continued).
Fig.2 shows elastic intensity and setting relative pressure of the water vapor to the time. The elastic
intensity increased with increasing the relative pressure. This result indicated that the water vapor
introduction succeeded. The recorded date at p / p0 = 1.0 were also sliced each 1 or 2h in order toevaluate the time evolution of the QENS patters.

Fig. 3. QENS profile at p / p0 = 1.0 after 12 h.

Fig. 4. Plot of intensities of the Lorentz
function for the fast mode on 0.5 and 12 h.

Fig. 3 shows QENS profile at p / p0 = 1.0 after 12 h. The time width was 2h. The enough statistics toanalyze the data was obtained. The profile was well fitted by sum of a delta function, two Lorentz
functions corresponding slow and fast modes, respectively and constant background convoluted withthe resolution function. The Q dependence of the half width at half maximum of the both modes wasalmost constant in the measured Q range (not shown here) and the observed modes might be due tothe localized mode. Fig. 4 shows Q dependence of the intensity of the Lorentz function for the fastmode. The data were fitted by the first-order spherical Bessel function in order to evaluate the intensity.
The obtained pre-factor of the fitted function was shown in Fig. 5. The intensity of the fast-mode
corresponding to the motion of the free water was saturated after 6 h otherwise, the intensity of the slow
mode corresponding to the confined water continued to increase. This result indicated that the structureof the hydrophilic domain keep changing during the adsorption in measured time range.

Fig. 5. Time evolution of the pre-factor of the sphericalBessel function for the slow and fast modes.
必要に応じて、A4 サイズの用紙に続きを記入して下さい。
Please use A4-size papers for further reporting, if necessary.