Analysis Results

General Information

Analysis date 2020/03/12 11:42:27

Sample name Measurement date 2020/03/12 11:27:13
File name H2SO4 14M 9V_Theta_2-Theta.raw Operator administrator
Comment

Measurement profile

Meas. data:H2SO4 14M 9V_Theta_2-Thet

a

300
Intensity (cps)

200

100

0
20 40 60 80
2-theta (deg)

-1-
Measurement conditions

X-Ray 30 kV , 10 mA Scan speed / Duration time 10.0000 deg./min.

Goniometer Step width 0.0200 deg.
Attachment - Scan axis 2Theta/Theta
Filter None Scan range 5.0000 - 80.0000 deg.
CBO selection slit - Incident slit -
Diffrected beam mono. None Length limiting slit -
Detector SC-70 Receiving slit #1 -
Scan mode CONTINUOUS Receiving slit #2 -

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Qualitative analysis results

Phase name Formula Figure of merit Phase reg. detail DB card number
Sulfuric_acid_octahydrate H2SO4.8H2O 1.895 User (COD) 2300373

Phase name Formula Space group Phase reg. detail DB card number
Sulfuric_acid_octahydrate H2SO4.8H2O 5 : I121,unique-b,cell-3 User (COD) 2300373

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 Meas. data:H2SO4 14M 9V_Theta_2-Thet
a

300
Intensity (cps)

200

100

0
Sulfuric_acid_octahydrate, H2SO4.8H2O, 2300373
20 40 60 80
2-theta (deg)

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Peak list

No. 2-theta(deg) d(ang.) Height(cps) FWHM(deg) Int. I(cps deg) Int. W(deg) Asym. factor
1 14.00(4) 6.323(19) 62(23) 0.83(13) 70(8) 1.1(6) 2(2)
2 16.50(11) 5.37(3) 72(25) 0.68(11) 63(9) 0.9(4) 1.7(16)
3 24.43(18) 3.64(3) 39(18) 6.1(5) 303(24) 8(4) 0.31(18)
4 63.63(15) 1.461(3) 9(9) 0.9(4) 9(5) 0.9(14) 0.3(12)
5 69.3(8) 1.355(13) 4(5) 4(2) 17(9) 5(10) 0.7(17)

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Parameters used for WPPF
Profile parameters

Common parameter Background Data H2SO4 14M 9V_Theta_2-Theta

Function name B-spline
param0 65.662885929243942
param1 59.585490680969144
param2 88.710113967307592
param3 104.46910981022586
param4 214.93909885439035
param5 123.31646718672961
param6 99.797947533675099
param7 93.556729522311628
param8 74.938396937737281
param9 67.677403345435039
param10 62.60358865678576
param11 68.640151750908444
param12 42.177560414854874
param13 61.479075784227234
node0 5
node1 11.16
node2 17.32
node3 24.640000000000001
node4 31.960000000000001
node5 39.280000000000001
node6 45.740000000000002
node7 52.200000000000003
node8 58.659999999999997
node9 65.159999999999997
node10 72.560000000000002
node11 80
Common parameter Peak shift
Function name Shift axial displacement
param0 0.099999291747691843
param1 0

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 param2 0
Sulfuric_acid_octahydrate Scale factor s 0.8(7)
FWHM U 5(62)
V 0(138)
W 3.9(15)
Asym. factor A0 -1.3(3)
A1 0(9)
Decay rate factor etaL0/mL0 0.1(19)
etaL1/mL1 -1(20)
etaL2/mL2 0.0000
etaH0/mH0 0.0(5)
etaH1/mH1 -1(11)
etaH2/mH2 0.0000
Preferred orientationMarch-Dollase h 0
k 0
l 0
March coefficient 1.000000

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Structure parameters

Data set name Phase Name Element x y z Occupancy Temperature factor

H2SO4 14M Sulfuric_acid_octah S 0.994370 0.163320 0.876620 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.768690 0.076690 0.832510 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 1.170080 0.017000 0.907670 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 1.060490 0.260600 0.838220 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.974830 0.321960 0.910370 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.111900 0.613000 0.853800 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.184000 0.726000 0.142100 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.210800 0.850000 0.008500 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.342400 0.479000 0.009200 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.090700 0.814000 0.397400 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.983100 0.505000 0.396100 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.074000 0.108000 0.744700 1.000 30.000
9V_Theta_2-Theta
H2SO4 14M ydrate
Sulfuric_acid_octah O 0.380740 0.239000 0.743300 1.000 30.000
9V_Theta_2-Theta ydrate

Data set name Rwp Rp Re S Chi^2 Maximum shift/e.s.d.

H2SO4 14M 29.12 22.51 27.19 1.0707 1.1464 0.297
9V_Theta_2-Theta

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Lattice constants
Angular correction

Analysis results

Data set name a(A) b(A) c(A) alpha(deg) beta(deg) gamma(deg)

H2SO4 14M 6.94(11) 7.3(5) 25.3(3) 90.000000 115.0(10) 90.000000
9V_Theta_2-Theta
Phase name a(A) b(A) c(A) alpha(deg) beta(deg) gamma(deg) V(A^3)
Sulfuric_acid_octah 6.94(11) 7.3(5) 25.3(3) 90.000000 115.0(10) 90.000000 1163(84)
ydrate
26
24
22
20
18
Lattice constants (ang.)

16
14
12
10
8
6
4
2
0
H2SO4 14M 9V_Theta_2-Theta
Data set

a b

-9-
Crystallinity

Data set name Crystallinity(%)

CrystallinityGraph.emf

- 10 -
Crystallite size and lattice strain
Williamson-Hall method

Data set name Crystallite size(A) Strain(%)

H2SO4 14M 9V_Theta_2-Theta 44.27(5) 0.82(10)

Phase name Crystallite size(A) Distribution RSD Strain(%) Distribution type

Sulfuric_acid_octahy 44.27(5) - 0.82(10) -
drate
CSSGraph.emf

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Quantitative analysis results (RIR)

RIRGraph.emf

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Quantitative analysis results (WPPF)

Phase name Content(%)

- Sulfuric_acid_octahydrate 100(90)

- 13 -
Quantitative analysis results (standard addition method)
Calibration data
QuantityCalibration.emf

- 14 -
Quantitative analysis results (External Standard method)
Calibration data
QuantityCalibration.emf

- 15 -
Quantitative analysis results (internal standard method)
Calibration Data
QuantityCalibration.emf

- 16 -
Stress
Stress constants

Analytical conditions

Analysis results

StressGraph.emf

- 17 -
Cluster analysis results
Dendrogram

ClusterDendrogram.emf

Measurement profiles

Meas. data:H2SO4 14M 9V_Theta_2-Thet

a

300
Intensity (cps)

200

100

0
20 40 60 80
2-theta (deg)

Cluster

Sample well

- 18 -
ClusterSamplePlate.emf

PCA view
ClusterPCA3DGraph.emf
Eigenvalue graph
ClusterPCAGraph.emf

- 19 -
Crystallite size distribution analysis results
Crystallite size distribution

Crystallite size distribution graph

1.0

0.8
Density function

0.6

0.4

0.2

0.0
0.0 0.2 0.4 0.6 0.8 1.0
Crystallite size(ang.)

- 20 -
Crystal structure analysis results
Indexing

Phase name Formula Figure of merit Phase reg. detail DB card number
Sulfuric_acid_octahydrate H2SO4.8H2O 1.895 User (COD) 2300373

Quantitative analysis results

Phase name Content(%)
- Sulfuric_acid_octahydrate 100(90)

Lattice information
Phase name a(A) b(A) c(A) alpha(deg) beta(deg) gamma(deg) V(A^3)
Sulfuric_acid_octah 6.94(11) 7.3(5) 25.3(3) 90.000000 115.0(10) 90.000000 1163(84)
ydrate
Phase name Space group Z Z' Calc. density(g/cm^3)
Sulfuric_acid_octahydrate 5 : I121,unique-b,cell-3 4 1.000 1.207

Structure determination

Refinement
Measurement range: 5.0000-80.0000deg Refinement range: 5.0000-80.0000deg (1.20 A)
Number of refined parameters: 29
Phase name Atomic coords # of indep. reflns
Sulfuric_acid_octahydrate Fractional coords 415

Rwp = 29.12% S = 1.0707

- 21 -
Crystal structure
CrystalGraph.emf

- 22 -