Intensity (counts) Intensity (counts)

Comment
File name
Analysis date
Sample name

-400
-200
1000
2000

200
400

0
0
General Information

Measurement profile

10
[1], d=8.74(13), 2-theta=10.11(16), H=10(3), Rel.H=0.45%
[2], d=7.497(4), 2-theta=11.795(7), H=564(24), Rel.H=24.76%

20
[3], d=4.2497(14), 2-theta=20.886(7), H=523(23), Rel.H=22.98%
[4], d=3.7743(18), 2-theta=23.552(12), H=86(9), Rel.H=3.75%

[5], d=3.2419(13), 2-theta=27.490(11), H=76(9), Rel.H=3.34%

[6], d=3.1540(7), 2-theta=28.272(

30
[8], d=2.8595(6), 2-theta=31.254(6), H=230(15), Rel.H=10.08%[9], d=2.80532(16), 2-thet
[10], d=2.7757(8), 2-theta=32.223(9), H=44(7), Rel.H=1.93%
[11], d=2.6719(5), 2-theta=33.511(6),
NaCl + CaSO4

[12], d=2.5830(18), 2-theta=34.70(2), H=27(5), Rel.H=1.18%

[13], d=2.4846(3), 2-theta=36.121(5),
NacL + CaSO4.raw
2016/08/19 15:29:56

2-theta (deg)
40
[15], d=2.2110(5), 2-theta=40.778(10), H=74(9), Rel.H=3.26%
[16], d=2.0788(3), 2-theta=43.498(8), H=79(9), Rel.H=3.48%[17], d=2.0673(8), 2-theta=43.752(
[18], d=2.0416(11), 2-theta=44.33(2), H=21(5), Rel.H=0.94%
[19], d=1.9883(2), 2-theta=45.586(5),
[21], d=1.8932(5), 2-theta=48.015(12), H=71(8), Rel.H=3.10%[22], d=1.8757(4), 2-theta=48.494(
[23], d=1.8602(5), 2-theta=48.924(13), H=14(4), Rel.H=0.61%

50
[24], d=1.80650(13), 2-theta=50.478(4
[26], d=1.7736(4), 2-theta=51.483(12), H=42(6), Rel.H=1.84%
[27], d=1.6959(3), 2-theta=54.028(9), H=18(4), Rel.H=0.77%
[28], d=1.6609(12), 2-theta=55.26(4), H

-1-
[30], d=1.58189(18), 2-theta=58.279(7), H=19(4), Rel.H=0.83%

60
Operator

[31], d=1.4364(5), 2-theta=64.86(2), H=19(4), Rel.H=0.82%

[32], d=1.40734(9), 2-theta=66.368(5), H
[33], d=1.3632(4), 2-theta=68.81(2), H=23(5), Rel.H=1.03%
Analysis Results

Measurement date

70
USER
2016/08/19 14:52:08
Measurement conditions

X-Ray 40 kV , 30 mA Scan speed / Duration time 4.0000 deg./min.

Goniometer Step width 0.0200 deg.
Attachment - Scan axis 2theta/theta
Filter K-beta filter Scan range 3.0000 - 70.0000 deg.
CBO selection slit - Incident slit 1/2 deg.
Diffrected beam mono. Length limiting slit -
Detector Scintillation counter Receiving slit #1 1/2 deg.
Scan mode CONTINUOUS Receiving slit #2 0.3mm

-2-
Qualitative analysis results

Phase name Formula Figure of merit Phase reg. detail DB card number
Gypsum Ca ( S O4 ) ( H2 O )2 0.763 ICDD (PDF-2 Release 2015 RDB) 01-076-8726
Halite, syn Na Cl 1.190 ICDD (PDF-2 Release 2015 RDB) 01-072-1668

Phase name Formula Space group Phase reg. detail DB card number
Gypsum Ca ( S O4 ) ( H2 O )2 15 : C12/c1,unique-b,cell-1 ICDD (PDF-2 01-076-8726
Halite, syn Na Cl 225 : Fm-3m Release 2015 RDB)
ICDD (PDF-2 01-072-1668
Release 2015 RDB)

-3-
 Integrated Intensity (counts deg) Intensity (counts)

1000
2000

100
200
300
400
500

0
0

10
Ca ( S O4 ) ( H2 O )2

Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2

20
Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2
Na Cl
Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2

30
Ca ( S O4 ) ( H2 O )2Ca ( S O4 )Na ( H2
Cl O )2Ca ( S O4 ) ( H2 O )
Ca ( S O4 ) ( H2 O )2Ca ( S O4 ) ( H2 O )2Ca ( S O4 ) ( H2 O
Ca ( S O4 ) ( H2 O )2Ca ( S O4 ) ( H2 O )2
( S O4 ) ( H2 O )
CaCa( S( SO4 O4) () H2
( H2OO)2)2Ca ( S O4 ) ( H2Ca O )2
Ca ( S O4 ) ( H2 O )2 Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2 Ca ( S O4 ) ( H2 O )2

2-theta (deg)
40
Ca ( S O4 ) ( H2 O )2

-4-
Ca ( S O4 ) ( H2 O )2
Ca ( S O4 Ca () S ( H2O4O) ()2Ca
H2 O( S )2O4
Ca () S ( H2O4O) ()2H2 O )2
Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2
NaCaCl( S O4 ) ( H2 O )2
Ca
Ca (( SS O4O4 )) (( H2H2 O )2Ca ( S O4 ) ( H2 O )2
O )2
Ca ( S O4 ) ( H2 O )2 )2Ca
Ca ( S O4O4 ) ( H2 O O )2
Ca (( SS O4 )) (( H2 H2 O )2)2Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2
50

Ca Ca ( S O4 ) (
)2Ca ( S O4 ) ( H2 O )2 H2 O )2Ca ( S O4 ) ( H2 O )2
CaCa(( S( SO4
S O4 ( H2O
O4)) ()( H2
H2 OO)2)2Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2Ca Ca (( SS O4
O4 )) (( H2 H2 O )2
O )2
Na Cl Ca ( S O4 ) ( H2 O )2
Ca Ca( S O4( S O4
) ( H2 ) ( H2
O )2OCa)2Ca ( S O4 ) ( H2 O )2
Cl ( S O4 ) ( H2 O )2
Ca Ca
( S (Na S O4
O4 ) ( H2 ) ( H2
O )2O )2Ca ( S O4 ) ( H2 OCa )2 ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2Ca (S
( S O4
O4 )) (( H2H2 O O )2
)2
Ca ( S O4 ) ( H2 O )2Ca Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2
60

CaCa (
Ca( (SSO4S O4 )
O4) )( (H2 ( H2 O )2
H2OO)2)2Ca Ca O4O4 H2
(H2 OO )2
)2
Ca Ca ( (S(SS
O4 ) )()(H2 O )2 Ca ( S O4 ) ( H2 O )2
Ca (( S S O4
O4 )) (( H2 H2 O O )2Ca
)2Ca (( SS O4
O4 )) (( H2 H2 OO )2Ca
)2 ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2Ca ( S O4 ) ( H2 O )2Ca Ca (( SS O4 )) (( H2
H2 O )2
O )2
Ca Ca
Ca ((SSO4
O4 O4 H2
((H2 O O)2 )2Ca
O)2Ca
Ca ( ((S
S O4 O4
SO4 ) ())H2 H2
((H2O OO)2
)2Ca)2 ( S O4O4 ) ( H2 O )2
Ca
CaNa
(( S
S O4 )) (())H2
H2
( SClO4 ) ( H2 O )2Ca O )2 ( S O4 ) ( H2 O )2 ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2Ca Ca ( S O4 ) ( H2 O )
Ca ( S O4 ) ( H2 O )2
Ca ( S O4 ) ( H2 O )2Ca ( S O4 ) ( H2 O )
*Optimized pattern is displayed.
70
Peak list

No. 2-theta(deg) d(ang.)

1 10.11(16) 8.74(13)
2 11.795(7) 7.497(4)
3 20.886(7) 4.2497(14)
4 23.552(12) 3.7743(18)
5 27.490(11) 3.2419(13)
6 28.272(7) 3.1540(7)
7 29.270(5) 3.0486(5)
8 31.254(6) 2.8595(6)
9 31.8738(19) 2.80532(16)
10 32.223(9) 2.7757(8)
11 33.511(6) 2.6719(5)
12 34.70(2) 2.5830(18)
13 36.121(5) 2.4846(3)
14 36.740(17) 2.4442(11)
15 40.778(10) 2.2110(5)
16 43.498(8) 2.0788(3)
17 43.752(18) 2.0673(8)
18 44.33(2) 2.0416(11)
19 45.586(5) 1.9883(2)
20 46.594(12) 1.9476(5)
21 48.015(12) 1.8932(5)
22 48.494(12) 1.8757(4)
23 48.924(13) 1.8602(5)
24 50.478(4) 1.80650(13)
25 50.867(6) 1.79358(19)
26 51.483(12) 1.7736(4)
27 54.028(9) 1.6959(3)
28 55.26(4) 1.6609(12)
29 56.633(18) 1.6239(5)
30 58.279(7) 1.58189(18)
31 64.86(2) 1.4364(5)
32 66.368(5) 1.40734(9)

-5-
33 68.81(2) 1.3632(4)

-6-
Parameters used for WPPF
Profile parameters

Common parameter Background Data NacL + CaSO4

Function name B-spline
param0 138.1161941339976
param1 138.24001873188746
param2 46.565610267638363
param3 63.784784051444511
param4 31.651166994602804
param5 36.428251263190724
param6 45.150859760914429
param7 19.215530495417021
param8 33.575970979682296
param9 22.977103161099901
param10 27.421414815546107
param11 22.331844290588979
param12 24.896000512800729
param13 16.83635570272731
param14 39.062413135794401
param15 14.957227060292777
param16 21.28267765176501
node0 3
node1 10.44
node2 17.879999999999999
node3 25.32
node4 30.16
node5 35
node6 39.840000000000003
node7 44.719999999999999
node8 48.82
node9 52.920000000000002
node10 57.020000000000003
node11 60.259999999999998
node12 63.5

-7-
 node13 66.739999999999995
node14 70
Common parameter Peak shift
Function name Shift axial displacement
param0 0
param1 0
param2 0
Gypsum Scale factor s 4.47(17)
FWHM U 0.0000
V -0.0039
W 0.0125
Asym. factor A0 0.8634
A1 1.5797
Decay rate factor etaL0/mL0 0.8765
etaL1/mL1 -0.3748
etaL2/mL2 0.0000
etaH0/mH0 0.4520
etaH1/mH1 0.3179
etaH2/mH2 0.0000
Preferred orientationMarch-Dollase h 0
k 0
l 0
March coefficient 1.000000
Halite, syn Scale factor s 6.7(17)
FWHM U 0.7145
V -0.4545
W 0.0784
Asym. factor A0 0.4353
A1 0.2729
Decay rate factor etaL0/mL0 0.7768
etaL1/mL1 -0.3679
etaL2/mL2 0.0000
etaH0/mH0 0.8685
etaH1/mH1 -0.3679
etaH2/mH2 0.0000
Preferred orientationMarch-Dollase h 0
k 0

-8-
 l 0
March coefficient 1.000000

-9-
Structure parameters

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

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

NacL + CaSO4 0 0 0 0 0 0

- 10 -
Lattice constants
Angular correction

Analysis results

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

NacL + CaSO4 6.260504 15.119482 5.657323 90.000000 114.099998 90.000000
NacL + CaSO4 5.615583 5.615583 5.615583 90.000000 90.000000 90.000000

Phase name a(A) b(A) c(A) alpha(deg) beta(deg) gamma(deg) V(A^3)

Gypsum 6.260504 15.119482 5.657323 90.000000 114.099998 90.000000 488.820124
Halite, syn 5.615583 5.615583 5.615583 90.000000 90.000000 90.000000 177.086154

16
15
14
13
12
11
Lattice constants (ang.)

10
9
8
7
6
5
4
3
2
1
0

NacL + CaSO4 NacL + CaSO4

Data set

a b c

- 11 -
Crystallinity

Data set name Crystallinity(%)

CrystallinityGraph.emf

- 12 -
Crystallite size and lattice strain
Williamson-Hall method

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

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

Gypsum - - - -
Halite, syn - - - -

CSSGraph.emf

- 13 -
Quantitative analysis results (RIR)

RIRGraph.emf

- 14 -
Quantitative analysis results (WPPF)

- 15 -
Quantitative analysis results (standard addition method)
Calibration data
QuantityCalibration.emf

- 16 -
Quantitative analysis results (External Standard method)
Calibration data
QuantityCalibration.emf

- 17 -
Quantitative analysis results (internal standard method)
Calibration Data
QuantityCalibration.emf

- 18 -
Stress
Stress constants

Analytical conditions

Analysis results

StressGraph.emf

- 19 -
 Cluster
Intensity (counts) Intensity (counts)

Sample well
Dendrogram

-400
-200
1000
2000

200
400

0
0
ClusterDendrogram.emf

Measurement profiles
Cluster analysis results

10
[1], d=8.74(13), 2-theta=10.11(16), H=10(3), Rel.H=0.45%
[2], d=7.497(4), 2-theta=11.795(7), H=564(24), Rel.H=24.76%

20
[3], d=4.2497(14), 2-theta=20.886(7), H=523(23), Rel.H=22.98%
[4], d=3.7743(18), 2-theta=23.552(12), H=86(9), Rel.H=3.75%

[5], d=3.2419(13), 2-theta=27.490(11), H=76(9), Rel.H=3.34%

[6], d=3.1540(7), 2-theta=2

30
[8], d=2.8595(6), 2-theta=31.254(6), H=230(15), Rel.H=10.08%[9], d=2.80532(16),
[10], d=2.7757(8), 2-theta=32.223(9), H=44(7), Rel.H=1.93%
[11], d=2.6719(5), 2-theta=33.
[12], d=2.5830(18), 2-theta=34.70(2), H=27(5), Rel.H=1.18%
[13], d=2.4846(3), 2-theta=36.1

2-theta (deg)
40
[15], d=2.2110(5), 2-theta=40.778(10), H=74(9), Rel.H=3.26%
[16], d=2.0788(3), 2-theta=43.498(8), H=79(9), Rel.H=3.48%[17], d=2.0673(8), 2-theta=4
[18], d=2.0416(11), 2-theta=44.33(2), H=21(5), Rel.H=0.94%
[19], d=1.9883(2), 2-theta=45.5
[21], d=1.8932(5), 2-theta=48.015(12), H=71(8), Rel.H=3.10%[22], d=1.8757(4), 2-theta=
[23], d=1.8602(5), 2-theta=48.924(13), H=14(4), Rel.H=0.61%

50
[24], d=1.80650(13), 2-theta=5
[26], d=1.7736(4), 2-theta=51.483(12), H=42(6), Rel.H=1.84%

- 20 -
[27], d=1.6959(3), 2-theta=54.028(9), H=18(4), Rel.H=0.77%
[28], d=1.6609(12), 2-theta=55.2

[30], d=1.58189(18), 2-theta=58.279(7), H=19(4), Rel.H=0.83%

60

[31], d=1.4364(5), 2-theta=64.86(2), H=19(4), Rel.H=0.82%

[32], d=1.40734(9), 2-theta=66.36
[33], d=1.3632(4), 2-theta=68.81(2), H=23(5), Rel.H=1.03%
70
ClusterSamplePlate.emf

PCA view
ClusterPCA3DGraph.emf
Eigenvalue graph
ClusterPCAGraph.emf

- 21 -
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.)

- 22 -
Crystal structure analysis results
Indexing

Phase name Formula Figure of merit Phase reg. detail DB card number
Gypsum Ca ( S O4 ) ( H2 O )2 0.763 ICDD (PDF-2 Release 2015 RDB) 01-076-8726
Halite, syn Na Cl 1.190 ICDD (PDF-2 Release 2015 RDB) 01-072-1668

Quantitative analysis results

Lattice information
Phase name a(A) b(A) c(A) alpha(deg) beta(deg) gamma(deg) V(A^3)
Gypsum 6.260504 15.119482 5.657323 90.000000 114.099998 90.000000 488.820124
Halite, syn 5.615583 5.615583 5.615583 90.000000 90.000000 90.000000 177.086154

Phase name Space group Z Z' Calc. density(g/cm^3)

Gypsum 15 : C12/c1,unique-b,cell-1 4 0.500 2.339
Halite, syn 225 : Fm-3m 4 0.021 2.192

Structure determination

Refinement
Measurement range: 3.0000-70.0000deg Refinement range: 3.0000-70.0000deg (1.34 A)
Number of refined parameters: 0
Phase name Atomic coords # of indep. reflns
Gypsum - 104
Halite, syn - 6

Rwp = - S=-

- 23 -
Crystal structure
CrystalGraph.emf

- 24 -