CHMI 2316E - Lab Manual PDF

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INORGANIC CHEMISTRY I LABORATORY MANUAL

CHMI 2316E 2020

COURSE PROFESSOR

LAB TECHNOLOGIST

LOUIS MERCIER

FRANÇOIS BRUNET

COPYRIGHT LAURENTIAN UNIVERSITY th

10

Edition © 2020

Original Author

Yoginder N. Sadana

Pieter Waern

Edited by

François D. Brunet

st

1

Edition © prior to 2009 by Yoginder N. Sadana and Pieter Waern

nd

2

CHMI 2316

– Fall 2020

th

to 10

Edition © 2012 to 2020 by F. Brunet

1

TABLE OF CONTENTS

CONTACT INFORMATION................................................................................................................... 4 PERIODIC TABLE ................................................................................................................................ 5 LABORATORY SCHEDULE ................................................................................................................... 6 SAFETY REGULATIONS OF THE LABORATORY .................................................................................... 7 IMPORTANT SAFETY CONTACT NUMBERS ....................................................................................... 11 EQUIPMENT HAZARDS ..................................................................................................................... 12 CHEMICAL HAZARDS ....................................................................................................................... 16 CHEMICAL HAZARD ASSESSMENT ................................................................................................ 20 RULES OF THE LABORATORY ........................................................................................................... 22 FORMAT OF THE LABORATORY REPORT .......................................................................................... 26 CHEMICAL KIT ................................................................................................................................. 27 PERSONNEL LAB EQUIPMENT .......................................................................................................... 28 INTRODUCTION ............................................................................................................................... 29 ANION ANALYSIS ............................................................................................................................. 30 PROCEDURE 1: DILUTE H2SO4 TEST ............................................................................................... 31 PROCEDURE 2: CONCENTRATED H2SO4 TEST ................................................................................ 32 PROCEDURE 3: SPECIFIC IONS TESTS ............................................................................................ 33 CONFIRMATION TESTS ................................................................................................................. 34 SODIUM CARBONATE EXTRACT ................................................................................................... 35 SILVER NITRATE TESTS FOR ANIONS ............................................................................................. 37 CATION ANALYSIS ........................................................................................................................... 38 PREPARING A SOLUTION OF THE SAMPLE .................................................................................... 39 SEPARATION INTO GROUPS ......................................................................................................... 40 ANALYSIS OF GROUP 1

– SILVER GROUP ..................................................................................... 42

ANALYSIS OF GROUP 2

– COPPER/ARSENIC GROUP..................................................................... 43

ANALYSIS OF GROUP 3

– ALUMINUM/IRON GROUP .................................................................... 45

ANALYSIS OF GROUP 4

– ZINC GROUP ........................................................................................ 46

ANALYSIS OF GROUP 5

– CALCIUM GROUP ................................................................................. 47

ANALYSIS OF GROUP 6

– MAGNESIUM GROUP ........................................................................... 48 +

TEST FOR AMMONIUM (NH4 ) ...................................................................................................... 50

2

CHMI 2316

– Fall 2020

FLAME TESTING ........................................................................................................................... 51 REACTIONS OF COMMON ANIONS .................................................................................................. 53 2-

CARBONATE (CO3 ) ..................................................................................................................... 53 2-

SULPHITE (SO3 ) ........................................................................................................................... 53 2-

SULPHIDE (S ) .............................................................................................................................. 54 2-

THIOSULPHATE (S2O3 ) ................................................................................................................. 54 -

NITRITE (NO2 ) .............................................................................................................................. 55 -

ACETATE (CH3COO ) ..................................................................................................................... 55 -

CHLORIDE (Cl ) ............................................................................................................................. 56 -

BROMIDE (Br ) .............................................................................................................................. 57 -

IODIDES (I ) .................................................................................................................................. 57 -

NITRATE (NO3 ) ............................................................................................................................. 58 -

FLUORIDE (F ) ............................................................................................................................... 59 2-

TARTRATE (C4H4O6 ) .................................................................................................................... 59 2-

OXALATE (C2O4 ) ......................................................................................................................... 59 2-

SULPHATE (SO4 ) ......................................................................................................................... 61 2-

BORATE (BO3 ) ............................................................................................................................ 61 3-

PHOSPHATE (PO4 ) ...................................................................................................................... 61 -

THIOCYANATE (SCN ) ................................................................................................................... 61 REACTIONS OF COMMON CATIONS ................................................................................................ 62 +

2+

GROUP 1 CATIONS (Ag , Hg2 2+

GROUP 2 CATIONS (Pb

3+

GROUP 3 CATIONS (Fe

2+

, Hg

, Al

2+

GROUP 4 CATIONS (Co

2+

GROUP 5 CATIONS (Ca

, Ni

2+

+

2+

, Cu

3+

, Cr

2+

, Sr

2+

GROUP 6 CATIONS (Mg

3+

2+

, Pb

) ........................................................................................... 62

, Bi

, Bi

5+

2+

, Cd

, As

3+

, As

5+

2/4+

, Sn

3/5+

, Sb

) .............................. 62

; Zr and Ti are omitted) ............................................................ 65

2+

, Zn

2+

and Mn

2+

& Ba +

3+

) ............................................................................. 65

) .......................................................................................... 67 +

, Li , Na , K ) ........................................................................................ 67

APPENDIX A

– SOLUBILITY GUIDELINES ........................................................................................... 69

APPENDIX B

– LIST OF REAGENTS ................................................................................................... 70

LAB REPORT COVER SHEETS AND OBSERVATION PAGES ................................................................. 75

CHMI

2316 – Fall 2020

3

CONTACT INFORMATION

COURSE PROFESSOR NAME OFFICE EMAIL EXT

Dr. Louis Mercier F-359 [email protected] 2111

LABORATORY TECHNOLOGIST NAME OFFICE EMAIL EXT

4

François (Frank) Brunet S-316 [email protected] 2365

CHMI 2316

– Fall 2020

Periodic Table of the Elements

1

1

H

0.08988

1s

atomic number

4.002602

4.216

He

3

Li

0.53

[He]2s

4

2

melting point /K

2745 1560

Be

density /(g/cm3; g/L for gases)

1.848

1

[He]2s

lit hium

1

Na

0.971

[Ne]3s

12 1.738

1

19

1

K

336.4 0.862

[Ar]4s

20 1757

Rb

1.53

1.55

[Kr]5s

55 942.5 301.55

38 1657 1042

1.873

Cs [Xe]6s

56 2170 998 3.51

Fr [Rn]7s

1

f rancium

88 1413 973 5.0

2

[He]2s 2p

21

2

[Ar]4s 3d

4.50

1

2

[Ar]4s 3d

scandium

2

[Kr]5s 4d

71

2

Ba*

3675 1936

[Kr]5s 4d

174.9668

72

3

2

14

[Xe]6s 4f 5d

**

Ra

103

radium

2

14

[Rn]7s 5f 6d

14

3269 16.6

104

Rf

—

1

2

14

[Rn]7s 5f 6d

57

*

2

138.90547 3

La

6.7

2

[Xe]6s 5d

—

organic or inorganic. For these elements, the average, with decreas ed prec ision, is reported. The data presented herein is not copyrightable. This file is copyright Roy Jensen, 2012. This file may be freely distributed in unaltered form. Distribution of this file or extracts therefrom, in any form, for a fee is expres sly prohibited. Last revised 06.2016

89

**

3500±300

1323 10.07

1

[227.0278] 3

Ac 2

[Rn]7s 6d act inium

14

1

14

3

6.78

(3),4

Ce 2

1

[Xe]6s 4f 5d

—

90 11.70

4

Th

[Rn]7s 6d t horium

14

4

— —

140.90765 (3),(4)

2

[Xe]6s 4f

2

91 — 1873 15.40

Bh

—

2

Pa 2

60 3347 1294

5

7.00

3

Nd

1

prot act inium

4

Os 2

92

14

[Rn]7s 5f 6d

3

[Rn]7s 5f 6d uranium

61 3300 (est.)

6

1315 6.475

1

93 4175 913 20.45

Pm 5

2

[He]2s 2p

26.981539

Al

78

—

Mt

—

2

14

[Rn]7s 5f 6d

7

4

nept unium

150.36 2,(3)

Sm

7.54

2

1

94 3505 914 19.80

14

Pu

[Rn]7s 5f

6

plut onium

—

Ds

—

1

14

[Rn]7s 5f 6d

9

darmst adt ium

63 1800 1095

151.964 2,(3)

Eu

5.259

2

[Xe]6s 4f

19.32

7

95 13.6

Am 2

7

americium

Hg

13.546

10

2

14

[Xe]6s 4f 5d

gold

mercury

[280.164]

111 — —

Rg

—

1

14

[Rn]7s 5f 6d

—

10

2

157.25

64 7.895

3

Gd 2

7

[Xe]6s 4f 5d

96 — 1613 13.5

65 3503 1629

7

curium

(3),4

2

1

97 — — —

Bk 2

2

9

berkelium

1833±5 544.5

Pb 14

10

9.80 2

2

Nh 2

14

10

1

114 — 2

66 8.536

2973 1747

Dy

8.80

10

2

99

Cf

— —

2

[Rn]7s 5f

10

calif ornium

—

14

10

3

Er 2

[Xe]6s 4f

2

14

10

14

10

— 2

— — —

Tm

9.33

12

2

[Xe]6s 4f

Fm [Rn]7s 5f

einst einium

f ermium

2

1469 1092 6.98

13

10

12

— — —

2

— — —

14

[259.1010] 2,3

No

13

[Rn]7s 5f

mendelevium

nobelium

[Rn]7s 5f

2

14

2

14

10

[Rn]7s 5f 6d 7p

yt t erbium

Md

Og

— 5

2,(3)

102

6

provisional

— —

Yb 2

10

[294]

118

173.054

[258.0984] 2,3

14

radon

14

[Xe]6s 4f

t hulium

101

2

[Xe]6s 4f 5d 6p

t ennessine

70

6

Rn

9.73 5

Ts

4

10

[222.0176] 0

86 211 202

provisional

— —

168.93421 2,(3)

69 2223 1818

2

[294]

117

livermorium

[257.0951] 3

11

[Rn]7s 5f

2

0

xenon

ast at ine

—

—

3

Xe

[Kr]5s 4d 5p

At

— 4

Lv

erbium

100

Es

10

[293]

— —

131.293

5

[209.9871] (±1),3,5,7

610 575

6

166.1 161.3

iodine

14

116

167.259

9.05

11

[252.0830] (2),3

2

2

10

[Kr]5s 4d 5p

85

10

54 5.88

[Xe]6s 4f 5d 6p [Xe]6s 4f 5d 6p

moscovium

Ho

holmium

2

Kr 2

[Ar]4s 3d 4p krypt on

[Rn]7s 5f 6d 7p [Rn]7s 5f 6d 7p [Rn]7s 5f 6d 7p

68

[Xe]6s 4f

4

polonium

provisional

2

10

0

3.708

5

I

387 4.93

Po

9.4 3

36 116.6

(±1),5,7

457.35 (35 ba r)

[208.9824] 2,(4)

84 1235 527

[288]

— 2

3141 1802

10

[251.0796] (3),4

2

10

83.798

120.9

126.90447

53

t ellurium

Mc

164.93032 3

dysprosium

98 —

67

3

[Xe]6s 4f

— —

10

f lerovium

162.500

2

14

[Rn]7s 5f 6d 7p

115

2

[Ar]4s 3d 4p

-2,(4),6

[Kr]5s 4d 5p

Bi 14

— —

Fl

nihonium

2840 1685

—

— —

Te

bismut h

[289.187]

3.119

6

argon

bromine

127.60

3

208.98040 (3),5

83

lead

[Rn]7s 5f 6d 7p

9

[247.0703] (3),4

[Rn]7s 5f

1

10

2

[Ne]3s 3p

Br

266

4

1263.1 722.7

ant imony

(2),4

11.34

10

provisional

—

10

t erbium

Cm 2

113

158.925

[Xe]6s 4f

14

[285]

— —

Tb

8.27

2

[Kr]5s 4d 5p

[Xe]6s 4f 5d 6p [Xe]6s 4f 5d 6p [Xe]6s 4f 5d 6p

copernicium

1

[247.0704] (3),4

[Rn]7s 5f 6d

14

[Rn]7s 5f 6d

roent genium

3546 1586

Cn

2

207.2

t hallium

—