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Prof John Dean

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Practical Skills in Chemistry John R. Dean • Alan M. Jones • David Holmes
John R. Dean • Alan M. Jones • David Holmes
Rob Reed • Jonathan Weyers • Allan Jones Rob Reed • Jonathan Weyers • Allan Jones
If you are studying chemistry, or a chemistry-related course, then this book will be an
indispensable companion throughout your entire degree programme. This ‘one-stop’ text will
guide you through the wide range of practical, analytical and data-handling skills that you will
need during your studies. It will also give you a solid grounding in wider transferable skills such Practical Skills in
Chemistry
as teamwork, using information technology, communicating information and study skills.
Chemistry
Practical Skills in
Now in its third edition, Practical Skills in Chemistry, 3e, has been enhanced and updated
throughout to provide a complete and easy-to-read guide to the developing skills required
from your first day through to graduation, further strengthening its reputation as the practical
resource for students of chemistry and related discipline areas.
This edition provides:

• New content layout to aid readability.
• ‘One-stop’ guide to the key practical skills needed in chemistry. THIRD EDITION
• Information presented in a clear and user friendly manner, tailored directly for the mastery of
basic laboratory skills.
• Numerous margin tips and hints, ‘how to’ boxes, checklists, worked examples and study
exercises.
• Guidance on numerical aspects, including statistics.
• Chapters grouped into key topics.
• Fully updated guide to health and safety, project work, Raman spectroscopy, internet
resources and enhancing your CV.
• New chapters on molecular formulae and X-ray diffraction.
• Generic guidance regarding Microsoft Office software, rather than version-specific details.
Practical Skills in Chemistry, 3rd edition, is an indispensable book for undergraduate

students in chemistry and related discipline areas and a useful primer for post-graduate
students. It is also a valuable resource for teachers in secondary schools.
THIRD
John R. Dean is Professor in Analytical and Environmental Sciences at the University of
Northumbria at Newcastle.
EDITION
Alan M. Jones was Head of Chemical Sciences at the University of Northumbria at Newcastle.
Reed • Weyers • Jones

Dean • Jones • Holmes
David Holmes is Associate Dean of the Keith B. Taylor Global Scholars Programme,
St George’s University School of Medicine (Grenada), based at the University of Northumbria at
Newcastle.
Rob Reed is Adjunct Professor (Education & Science) at Central Queensland University,
Australia.
Jonathan Weyers is Honorary Senior Lecturer at the University of Dundee.
Allan Jones is the Chancellor’s Award Fellow in Ecology, Environmental Science and Zoology
at the University of Dundee.
Cover image: Michael Rozewski/Getty Images www.pearson-books.com
CVR_DEAN_03_39920.indd 1 02/05/2017 14:01

Practical Skills in Chemistry
A01 Practical Skills in Chemistry 39920.indd 1 11/05/2017 09:13

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Practical Skills in Chemistry
Third Edition
John R. Dean
Alan M. Jones
David Holmes
Rob Reed
Jonathan Weyers
Allan Jones
Harlow, England • London • New York • Boston • San Francisco • Toronto • Sydney • Dubai • Singapore • Hong Kong
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First published 2002 (print)

Second edition published 2011 (print and electronic)
Third edition published 2017 (print and electronic)
© Pearson Education Limited 2002 (print)

© Pearson Education Limited 2011, 2017 (print and electronic)
The rights of John R. Dean, Alan M. Jones, David Holmes, Rob Reed, Jonathan Weyers and Allan Jones
to be identified as authors of this work have been asserted by them in accordance with the Copyright,
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ISBN: 978-1-292-13992-0 (print)

978-1-292-13993-7 (PDF)
978-1-292-13994-4 (ePub)
British Library Cataloguing-in-Publication Data

A catalogue record for the print edition is available from the British Library
Library of Congress Cataloging-in-Publication Data

Names: Dean, John R.
Title: Practical skills in chemistry.
Description: Third edition / John R. Dean [and five others]. | Harlow,
England : Pearson, 2017. | Includes bibliographical references and index.
Identifiers: LCCN 2017002095| ISBN 9781292139920 (print) | ISBN 9781292139937
(pdf) | ISBN 9781292139944 (epub)
Subjects: LCSH: Chemistry--Study and teaching.
Classification: LCC QD33.2 .P73 2017 | DDC 542--dc23
LC record available at https://lccn.loc.gov/2017002095
10 9 8 7 6 5 4 3 2 1
21 20 19 18 17
Print edition typeset in 10/12pt Times LT Pro by Spi Global

Printed and bound in Malaysia
NOTE THAT ANY PAGE CROSS REFERENCES REFER TO THE PRINT EDITION

Contents
List of boxes viii

Preface to the third edition xi
Guided tour xii
For the student xiv
Acknowledgements xv
List of abbreviations xvi
The investigative approach 1

1. Essentials of practical work 3
2. Health and safety 6
3. Making measurements 36
4. SI units and their use 40
5. Scientific method and design of experiments 46
6. Making notes of practical work 52
7. Project work 56
Fundamental laboratory techniques 61

8. Working with liquids 63
9. Basic laboratory procedures I 70
10. Basic laboratory procedures II 82
11. Principles of solution chemistry 102
12. pH and buffer solutions 113
Laboratory techniques 121

13. Melting points 123
14. Recrystallisation 128
15. Solvent extraction 139
16. Distillation 145
17. Reflux 155
18. Evaporation 161
19. Inert atmosphere methods 166
20. Combinatorial chemistry 173
Classical techniques 177

21. Qualitative techniques for inorganic analysis 179
22. Gravimetry 184
23. Molecular formulae 187
24. Procedures in volumetric analysis 190
25. Acid–base titrations 199
26. Complexometric titrations 203
27. Redox titrations 208
28. Precipitation titrations 211

Contents
Instrumental techniques 215

29. Basic spectroscopy 217
30. Atomic spectroscopy 226
31. X-ray fluorescence spectroscopy 243
32. Chromatography 250
33. Electrophoresis 287
34. Electroanalytical techniques 302
35. Using radioisotopes 309
36. Infrared and Raman spectroscopy 318
37. Nuclear magnetic resonance spectrometry 332
38. Mass spectrometry 353
39. X-ray diffraction 362
40. Thermal analysis 370
Information technology and library resources 373

41. Finding and citing published information 375
42. Evaluating information 382
43. Using online resources 389
44. Internet resources 399
45. Using spreadsheets 421
46. Using word processors, databases and other packages 428
Analysis and presentation of data 435

47. Fundamental principles of quantitative chemical analysis 437
48. Calibration and quantitative analysis 441
49. Using graphs 447
50. Presenting data in tables 459
51. Hints for solving numerical problems 463
52. Manipulating and transforming raw data 472
53. Descriptive statistics 476
54. Choosing and using statistical tests 487
55. Drawing chemical structures 501
56. Chemometrics 507
57. Computational chemistry 514
Study and examination skills 521

58. The importance of transferable skills 523
59. Managing your time 529
60. Working with others 534
61. Taking notes from lectures and texts 538
62. Learning effectively 544
63. Revision strategies 551
64. Assignments and exams 556
65. Preparing your curriculum vitae 566
vi

Contents
Communicating information 573

66. Organising a poster display 575
67. Giving a spoken presentation 581
68. General aspects of scientific writing 587
69. Writing essays 594
70. Reporting practical and project work 597
71. Writing literature surveys and reviews 606
Answers to study exercises 609

Index 627
vii

List of boxes
2.1 How to perform a risk matrix analysis 8

4.1 Conversion factors between some redundant units and the SI 42
4.2 How to interconvert SI units 44
5.1 Checklist for designing and performing an experiment 49
7.1 How to write a project proposal 57
8.1 Using a pipettor to deliver accurate, reproducible volumes of liquid 66
9.1 How to make up an aqueous solution of known concentration from
a solid chemical 72
9.2 How to make up an aqueous solution of known concentration from
a solid chemical for use in quantitative analysis 74
9.3 How to make up a linear dilution series for use in quantitative analysis 77
9.4 How to weigh out a sample of a solid for use in quantitative analysis 80
10.1 How to flute a filter paper for gravity filtration 84
10.2 Isolation of a solid by suction filtration 86
10.3 How to dry a solution over magnesium sulphate 98
11.1 Useful procedures for calculations involving molar concentrations 103
11.2 How to convert ppm into mass of chemical required 104
11.3 An example of complex formation 108
11.4 The use of oxidation numbers to identify redox systems 110
11.5 How to balance redox equations from partial ionic equations using the
ion–electron method 110
12.1 Using a glass pH electrode and meter to measure the pH of a solution 115
14.1 How to carry out a solvent selection for recrystallisation of an unknown compound 131
14.2 How to carry out a mixed-solvent selection for recrystallisation
of an unknown compound 132
14.3 How to carry out a single-solvent recrystallisation 133
14.4 How to carry out a mixed-solvent recrystallisation 135
15.1 How to separate a carboxylic acid and a hydrocarbon using solvent extraction 142
15.2 How to set up a Soxhlet extraction system 143
16.1 How to assemble the apparatus for a simple distillation 147
16.2 How to carry out a simple distillation 147
16.3 How to carry out a fractional distillation 148
16.4 How to carry out a reduced-pressure distillation using a water pump 150
16.5 How to carry out a steam distillation 153
17. 1 How to set up a simple reflux apparatus 156
17. 2 How to set up the apparatus for reflux with mechanical stirring 157
18.1 How to use a rotary film evaporator 162
19.1 How to transfer an air-sensitive reagent using a syringe 170
21.1 How to use a low-speed bench centrifuge 181
22.1 How to carry out gravimetric analysis 184
23.1 How to calculate a molecular formula from microanalytical data 188
24.1 Types of calculations used in volumetric analysis – titrations 191
24.2 How to fill a pipette 195
24.3 How to carry out a titration 195
29.1 How to use a UV/visible spectrophotometer 220
29.2 How to use a flame photometer 223
30.1 How to prepare a 1000 mg mL-1 stock solution of a metal ion from a metal salt 226
30.2 How to prepare a set of five calibration solutions in the concentration range
0910 mg mL-1 (mg L-1) 227
30.3 How to analyse a sample using the method of standard additions in FAAS 229
30.4 Sample size and certified reference materials 229
viii

List of boxes
30.5 Analysis of a sample: dilution factor 230

30.6 How to operate a flame atomic absorption spectrometer 233
30.7 How to acid-digest a sample using a hot plate 240
31.1 How to avoid problems with liquid samples in XRF 247
31.2 How to prepare a loose powder sample for XRF analysis 249
32.1 How to prepare a set of five calibration solutions in the concentration range
0910 mg mL-1 (mg L-1) 257
32.2 How to make micropipettes for TLC 261
32.3 How to run a TLC 262
32.4 How to prepare and run a flash column 264
32.5 How to use a Soxtec extractor 273
32.6 Procedure for Shake Flask extraction 274
32.7 Procedure for ultrasonic extraction 275
32.8 How to operate a typical supercritical fluid extraction system 275
32.9 How to operate a typical pressurised microwave-assisted extraction (MAE) system 276
32.10 How to operate a typical pressurised fluid extraction (PFE) system 277
32.11 How to use a low-speed bench centrifuge 277
32.12 How to pre-concentrate a sample using a reversed phase C18 solid phase
extraction (SPE) cartridge 280
32.13 How to concentrate a sample of an organic compound in an aqueous sample
using direct solid phase microextraction (SPME) 281
32.14 How to concentrate a sample of an organic compound in an aqueous sample
using headspace solid phase microextraction (SPME) 281
33.1 How to carry out agarose gel electrophoresis of DNA 290
33.2 How to carry out SDS-PAGE for protein separation 294
35.1 How to determine the specific activity of an experimental solution 312
35.2 Tips for preparing samples for liquid scintillation counting 314
36.1 How to run an infrared spectrum of a liquid, solid film, mull or KBr disk 321
36.2 How to prepare liquid and solid films and mulls 323
36.3 How to prepare a KBr disk 324
36.4 How to interpret an IR spectrum 327
37.1 How to prepare a sample for NMR spectroscopy 335
37.2 How to interpret a 1H9 1H@COSY spectrum 349
38.1 How to identify the number of bromine or chlorine atoms in a molecule
from the molecular ion 355
38.2 Idealised fragmentation processes for the molecular ion (M +) 356
39.1 Press and Pull method for mounting of specimen 364
39.2 Back-loading method for mounting of specimen 364
39.3 Side-loading method for mounting of specimen 365
40.1 How to interpret a thermal analysis trace 371
42.1 How to avoid plagiarism and copyright infringement 383
43.1 Important guidelines for using PCs and networks 390
43.2 Getting to grips with e-learning 391
43.3 Useful tips for using search engines 394
43.4 Getting the most from Google searches 395
43.5 How to evaluate information on the Web 396
48.1 The stages involved in preparing and using a calibration curve 442
48.2 How to use a spreadsheet (a Microsoft Excel ) to produce a linear regression plot 444
49.1 Checklist for the stages in drawing a graph 450
49.2 How to create and amend graphs within a spreadsheet (Microsoft Excel )
for use in coursework reports and dissertations 450
49.3 How graphs can misrepresent and mislead 456
50.1 Checklist for preparing a table 460
50.2 How to use a word processor (Microsoft Word) or a spreadsheet (Microsoft Excel)
to create a table for use in coursework reports and dissertations 461
ix

List of boxes
5 1.1 Example of using the algebraic rules of Table 51.2 465

53.1 Descriptive statistics for a sample of data – an example 478
53.2 Three examples where simple arithmetic means are inappropriate 479
53.3 How to use a spreadsheet (Microsoft Excel) to calculate descriptive statistics 484
54.1 How to carry out a t-test 492
54.2 Worked example of a t-test 493
54.3 Using a spreadsheet (Microsoft Excel) to calculate hypothesis-testing statistics 497
56.1 Example of a two-level factorial design 509
56.2 Example of principal component analysis 512
58.1 How to carry out a personal skills audit 526
59.1 Tips for effective planning and working 532
61.1 The SQ3R technique for skimming texts 542
62.1 How to diagnose your learning preferences using the VAK scheme 546
62.2 How to accommodate different lecturers, teaching styles 548
63.1 How to use past exam papers in your revision 553
63.2 How to prepare and use a revision timetable 553
63.3 How to revise actively 554
64.1 Problem-based learning (PBL) 557
64.2 Writing under exam conditions 559
64.3 Reasons for poor exam answers to essay-style questions 560
64.4 Strategies for combating the symptoms of exam anxiety 564
65.1 The structure and components of a typical CV and covering letter 568
66.1 How to create a poster using Microsoft PowerPoint 579
67.1 Tips on preparing and using Microsoft PowerPoint slides in a spoken presentation 582
67.2 Hints on spoken presentations 585
68.1 How to achieve a clear, readable style 590
68.2 Using appropriate writing styles for different purposes (with examples) 591
68.3 How to improve your writing ability by consulting a personal reference library 592
70.1 The structure of reports of experimental work using the ‘IERaD’ structure 598
70.2 Writing experimental procedures 600
70.3 How to write up your research project (dissertation) or thesis 602
70.4 Steps in producing a scientific paper 604
71.1 How to analyse a topic using the SPSER approach 607

Preface to the third edition
‘Chemistry can be defined as the science that studies practical skills. Specifically, ‘to develop in students a range
systematically the composition properties, and reactivity of practical skills so that they can understand and assess
of matter at the atomic and molecular level. Since matter risks and work safely and competently in the laboratory’
is everything that can be touched, made visible, smelt or [for undergraduate students] and ‘to provide students with
tasted, it follows that the scope of chemistry as a subject the ability to plan and carry out experiments independently
is very broad’. and assess the significance of outcomes’ [for postgraduate
students].
To students who buy this book, we hope you will find
QAA for HE Subject Benchmark it useful in the laboratory during your practical classes and
Statement for Chemistry (2014). in your project work – this is not a book to be left on the
Practical skills form the cornerstone of chemistry. Howev- bookshelf.
er, the diversity of skills required in the laboratory means We would like to take this opportunity to thank our wives
that a student’s experience may be limited. While some and families for their continued support, and to recognise
techniques do require specific skills, many of them are the following colleagues and friends who have provided as-
transferable generic skills that are required throughout the sistance, comment and food for thought at various points
subject area. during the production of all editions: Gary Askwith, Dave
The time constraints of the modern curriculum often Bannister, Jon Bookham, Samantha Bowerbank, Susan
preclude or minimise laboratory time. It is the aim of this Carlile, Michelle Carlin, Jim Creighton, Sarah
Cresswell,
book to provide general guidance for use in and out of prac- Martin Davies, Mike Deary, Les Dix, M arcus Durrant,
tical sessions and also to cover a range of techniques from Jackie Eager, Gordon Forrest, Derek Holmes, Ed Ludkin,
the basic to the more advanced. Dave Osborne, Justin Perry, Lee Rounds, Jane Shaw, Tony
In creating the third edition of Practical Skills in Chem- Simpson, Dave Wealleans and Ian Winship. We would also
istry, we have maintained the approach of the previous like to thank the staff of Pearson Education for the friend-
editions, with the aim of providing support to students tak- ly support over the years, and would wish to acknowledge
ing chemistry based courses in a concise and user friendly Richelle Zakrewski, Rufus Cornow, Pat Bond, Owen Knight,
manner. Key points, definitions, illustrations, ‘how to’ box- Simon Lake, Alex Seabrook and Pauline Gillett.
es, checklists, worked examples, tips and hints are includ- As with previous editions, we would be grateful to
ed where appropriate. However, we have also used this hear of any errors you might notice, so that these can be
opportunity of the new edition to restructure the layout, put right at the earliest opportunity.
to literally start at the beginning of the laboratory process
and progress to the end, with the dissemination of results.
In updating and thoroughly revising the book to in-
clude a ‘taste’ of the latest developments in methodology, JOHN R. DEAN ([email protected])
we have considered carefully the Quality Assurance Agen- ALAN M. JONES ([email protected])
cy UK Subject Benchmarking statements for Chemistry, re-
viewed and updated in 2014, and have attempted to cover DAVE HOLMES ([email protected])
all of the generic skills, along with the practical aspects ROB REED ([email protected])
of the subject specific topics in chemistry. We have been
ALLAN M. JONES ([email protected])
mindful of two of the QAA’s aims for chemistry degree
(under- and post-graduate) programmes in the context of JONATHON WEYERS ([email protected])

xi

Guided tour
43 Using online resources
Information and communication technology (ICT) is vital in the modern aca-

Definitions demic world and ‘IT literacy’ is a core skill for all bioscientists. This involves
Definitions of key terms and

a wide range of computer-based skills, including:
Browser – a program to display web
pages and other Internet resources. ●● Accessing web pages using a ‘browser’ such as Internet Explorer, Firefox
Safari or Chrome.
concepts are highlighted in FAQ – Frequently Asked Question; a file
or web page giving information on com- ●● Searching the web for useful information and resources using a search
engine such as Google, or a meta-search engine such as Dogpile.
mon queries, sometimes used as a file
the text margin. extension (.faq).
FTP – File Transfer Protocol; a mecha-
●● Finding what you need using online databases, such as library catalogues
or complex websites, such as your university’s homepage.
nism for downloading files. ●● Downloading, storing and manipulating files.
URL – Uniform Resource Locator; the ●● Communicating via the Internet.
‘address’ for web resources.
●● Using e-learning facilities effectively.
●● Working with ‘Office’-type programs and other software (dealt with in
detail in Chapters 45 and 46).
Academic use of ICT resources – a
range of in appropriate activities will be You will probably receive an introduction to your university’s networked
identified in your university’s rules for IT systems and you will be required to follow rules and regulations that are
use of ICT systems. They may include: important for the operation of these systems. Whatever your level of experience
hacking, spamming, using another per- with PCs and the Internet, you should also follow the basic guidelines shown
son’s account, and copyright infringe- in Box 43.1. Reminding yourself of these from time to time will reduce your
ment, as well as broader aspects of chances of losing data.
behaviour covered by a code of conduct
or student charter The Internet as a global resource
The Internet is a complex network of computer networks; it is loosely organised
and no one group organises it or owns it. Instead, many private organisations,
universities and government organisations fund and operate discrete parts of it.
The web is the most popular application of the Internet. It allows easy
Tips and Hints provide use- links to information and files which may be located on networked computers
across the world. The web enables you to access millions of ‘homepages’ or
ful hints and practical advice,

‘websites’ – the initial point of reference with many individuals, institutions
and companies. Besides text and images, these sites may contain ‘hypertext
links’, highlighted words or phrases that take you to another Internet location
and are highlighted in the text Understanding the technology – you

do not need to understand the work-
via a single mouse click.
You can gain access to the Internet either through a network at your uni-
versity, at most public libraries, at a commercial ‘Internet cafe’, or from home
margin. ings of the Internet to use it – most of
it is invisible to the user. To ensure you
via a modem connected to a broadband or dial-up internet service provider
(e.g. Virgin Media, BT or Sky).
obtain the right facilities, you may need
to know some jargon, such as terms for
Key PoInT Most material on the Internet has not been subject
Key Points highlight critical
the speed of data transfer (megabits)
and the nature of internet addresses. to peer review or vetting. Information obtained from the web or
Setting up a modem and/or local posted on newsgroups may be inaccurate, biased or spoof; do
features of methodology. wireless network can be complex, but

instructions are usually provided with
not assume that everything you read is true, or even legal.
the hardware. White and Downs (2014) online communication

and Gralla (2006) are useful texts if you
wish to learn more about computing
You will be allocated an email account by your university and should use
and the Internet.
this routinely for communicating with staff and fellow students, rather than
using a personal account. You may be asked to use email to submit work as
Information technology and library resources 389
M43 Practical Skills in Chemistry 39920.indd 389 10/05/2017 20:22
Basic laboratory procedures I
35 Using radioisotopes Box 9.4 How to weigh out a sample of a solid for use in
quantitative analysis
The isotopes of a particular element have the same number of protons in the 1. Place the clean, dry weighing boat or sample tube on a general-
Examples 126 C, 136 C and 146 C are three of purpose two-decimal-place balance and zero the balance.
nucleus but different numbers of neutrons, giving them the same proton number
the isotopes of carbon. About 98.9% (atomic number) but different nucleon numbers (mass number, i.e. number of 2. Weigh out the calculated amount of chemical within the accuracy of
of naturally occurring carbon is in the
protons + number of neutrons). Isotopes may be stable or radioactive. Radi- the balance.
stable 126 C form. 136 C is also a stable
oactive isotopes (radioisotopes) disintegrate spontaneously at random to yield
isotope but it only occurs at 1.1% natu- 3. Check the zero reading on the analytical balance by pressing the bar/
ral abundance. Trace amounts of radio- radiation and a decay product. button with the balance doors closed.
active 146 C are found naturally; this is a
4. Relock the balance pan by pressing the bar/button.
negatron-emitting radioisotope. Radioactive decay
5. Carefully transfer the weighing boat or sample tube to the balance
There are three forms of radioactivity (Table 35.1) arising from three main
pan of the analytical balance (for very accurate work use tweezers
types of nuclear decay: or fine tongs since the sweat from your fingers will contribute to the
●● Alpha decay. This involves the loss of a particle equivalent to a helium weight recorded) and close the balance door.
Examples 226Ra decays to 222Rn by nucleus. Alpha (a) particles, being relatively large and positively charged,
loss of an alpha particle, as follows:
6. Release the balance pan by pressing the bar/button, allow the balance
do not penetrate far in living tissue, but they do cause ionisation damage and to stabilise and record the weight of the chemical and container. If the
226
88 Ra S 222 4
86 Rn + 2He
2+ this makes them generally unsuitable for tracer studies. last decimal place ‘cycles’ between two or three numbers, determine
the mid-point of the ‘cycle’ and record this value as the weight.
14
C shows beta decay, as follows: ●● Beta decay. This involves the loss or gain of an electron or its positive
14 S 147 N + b-
counterpart, the positron. There are three subtypes: 7. Lock the balance pan by pressing the bar/button, remove the sample
6C
container and transfer the solid to your volumetric flask, beaker or
22 (a) Negatron (b- ) emission: loss of an electron from the nucleus when
Na decays by positron emission, as conical flask by pouring, but do not wet the weighing boat or sample
follows: a neutron transforms into a proton. This is the most important form tube with solvent.
of decay for radioactive tracers used in chemistry. Negatron-emitting
22 S 22 +
11Na 10Ne + b isotopes of importance include 3H, 14C, 32P and 35S. 8. Replace the weighing container on the analytical balance pan, close
55 the balance door and weigh the container. Again decide on the mid-
Fe decays by electron capture and (b) Positron (b+ ) emission: loss of a positron when a proton transforms into point weight if the last decimal place ‘cycles’ and record this value
the production of an X-ray, as follows: a neutron. This only occurs when sufficient energy is available from as the weight of the ‘empty’ weighing container.
55
26Fe S 55
25Mn + X the transition and may involve the production of gamma rays when the
positron is later annihilated by collision with an electron. 9. Lock the balance pan by pressing the bar/button and remove the
The decay of 22Na by positron emis- weighing container from the balance.
sion (b+) leads to the production of a (c) Electron capture (EC): when a proton ‘captures’ an electron and trans- Fig. 9.5 Transferring a solid using glazed
g ray when the positron is annihilated paper. 10. Subtract the weight of the ‘empty’ weighing container from that of
forms into a neutron. This may involve the production of X-rays as
on collision with an electron. the weighing container plus sample and you now know the mass
electrons ‘shuffle’ about in the atom (as with 125I) and it frequently
of chemical, to an accuracy of four decimal places, which has been
involves electron emission.
transferred into your volumetric flask, beaker or conical flask.
●● Gamma emission. Internal transition involves the emission of electromag-
netic radiation in the form of gamma (g) rays from a nucleus in a metastable
state and always follows initial alpha or beta decay. Emission of gamma amounts of solid are to be transferred, it is advisable to use a wide-necked filter
folded glazed paper
radiation leads to no further change in atomic number or mass. funnel called a ‘powder funnel’.
solid In many preparative experiments, which are carried out on a small scale
Note from the above that more than one type of radiation may be emitted (involving 1 g to 10 g of solids), the most useful weighing container is spe-
when a radioisotope decays. The main radioisotopes used in chemistry and rolled glazed paper
cial glazed paper, provided that the chemicals do not react with the paper.
their properties are listed in Table 35.2. A creased square of glazed paper is ‘tared’ on the balance pan and the solid
weighed out directly onto it. The chemical can then be allowed to flow down
Table 35.1 Types of radioactivity and their properties. the crease into the vessel (Fig. 9.5). Furthermore, when attempting to transfer
small amounts of solid in vessels with narrow-bore ground-glass joints (see
Range of maximum Penetration range Suitable shielding flask p. 98) it is important not to allow the solid to contact the joint, because the joint
Radiation energies (MeV*) in air (m) material will not seal correctly. Use a filter funnel or roll a piece of glazed paper into
Alpha (a) 4–8 0.025–0.080 Unnecessary a funnel, insert the stem of the paper funnel to below the joint and then run in
the solid from the creased weighing paper (Fig. 9.6). Paper used in this manner
Beta (b) 0.01–3 0.150–16 Plastic (e.g. Perspex)
Fig. 9.6 Transferring a solid to a narrow-necked is much cheaper than proprietary weighing dishes and is a useful method of
Gamma (g) 0.03–3 1.3–13† Lead flask. recycling out-of-date manufacturers’ catalogues!
*Note that 1 MeV = 1.6 * 10 -13 J.
† Distance at which radiation intensity is reduced to half. 80 Fundamental laboratory techniques
Instrumental techniques 309
M35 Practical Skills in Chemistry 39920.indd 309 10/05/2017 19:58 Worked examples and ‘How to’ boxes
Examples are included in the margin to illustrate important set out the essential procedures in a
points without interrupting the flow of the main text. step-by-step manner.
xii

Guided tour
Chromatography
100% dimethylsiloxane:
the least polar bonded phase. Used for boiling point
separations (solvents, petroleum products, etc.).
Typical names: DB–1, HP–1, Rtx–1
CH3
Si O
CH3
Figures are used to illustrate (a) (b)
95% dimethylsiloxane–5% diphenylypolysiloxane:
key points, techniques and a non-polar phase. Used for separation of environmental
samples, e.g. polycyclic aromatic hydrocarbons.
Typical names: DB–5, HP–5, Rtx–5
equipment. CH3
Si O Si O
CH3
(c) (d) 5% 95%
Fig. 32.11 Sample injection in GC. (a) Fill the syringe, (b) wipe clean the Fig. 32.13 Common stationary phases for
Chromatography
outside of the syringe needle, (c) place the syringe needle into the injector capillary GC.
and (d) depress the plunger on the syringe to inject the sample.
Polyimide syringe
coating
Fused-silica PTFE block
Stationary
phase
syringe
Fig. 32.12 Schematic diagram of a GC column.

to purge
valve ball valve
septum
Box 32.1 How to prepare a set of five calibration solutions in the concentration range
0910 mg mL −1 (mg L -1)
syringe needle
glass liner
Assuming that we are starting with a 1000 mg mL-1 [32.9]
column end
stock solution of a particular organic compound (e.g.
carrier in the 10.00 mL
so 20 mg 2-chlorophenol was placed
2-chlorophenol) you will need the following: 6 * 10.00 mL gas inlet
grade A volumetric
column flasks and a syringe (09100.00 mL). volumetric flask. So,
compressed
1. ensure that all the glassware is clean (see p. 68). 20 mg air
= 2 mg mL-12 @chlorophenol
for cooling [32.10]
10 mL
2. Add ?9 mL of organic solvent (e.g. dichloromethane) inside the oven
carrier to split valve
to a 10.00 mL with dichloromethane.
gas inlet
You now have a 2 mg mL-1 calibration solution of
2-chlorophenol.
3. Quantitatively transfer 20.00 mL of the stock solu-
tion into the 10.00 mL volumetric flask. Inject the 5. Similarly transfer 0,syringe
40.00,needle
60.00, 80.00 and 100.00 mL
solution from the syringe below the surface of the volumes into separate volumetric flasks and dilute
dichloromethane. Then, dilute to 10.00 mL with to 10.00 mL with dichloromethane and label as 0,
(a) (b)
dichloromethane. 4, 6, 8 and 10 mg mL-1 2-chlorophenol calibration
Fig. 32.10 Sample introduction in GC: (a) split/splitless injector; (b) solutions.
on-column injector.
4. What is the concentration of this new solution?
Remember that we started with an initial 1000 mg mL-1 6. take the 0, 2, 4, 6, 8 and 10 mg mL-1 2-chlorophe-
2-chlorophenol stock solution. nol calibration solutions to the chromatograph for
1000 mg analysis.
* 20 * 10-3 mL = 20 mg 2@chlorophenol
Fig. 32.12: at normal operating temperatures. This behaves in a similar man-
mL compounds by GC in the
Analysing
ner to a liquid film, but is far more robust. Common stationary phases for GC
split mode – make sure no hazardous
are shown in Fig. 32.13. The mobile phase (‘carrier gas’) is usually nitrogen
materials enter the laboratory atmos- Instrumental techniques
or helium. Selective separation is achieved as a result of the differential parti- 257
phere through the split vent. A charcoal
tioning of individual compounds between the carrier gas and silicone polymer
split-vent trap may be required to elim-
phases. The separation of most organic molecules is influenced by the temper-
inate potential hazards.
ature of the column, which may be constant during the analysis (‘isothermal’ –
usually 50–250 °C) or, more commonly, may increase in a pre-programmed
M32 Practical Skills in Chemistry 39920.indd 257 manner (e.g. from 50 °C to 250 °C at 10 °C per min). 10/05/2017 19:49
Selecting an appropriate column for capillary GC is a difficult task and

SI units and their use one which is usually left to the technician. However, it is important to be Precipitation titrations
aware of some general issues and what influence they can have on the sep-
aration. The column internal diameter can affect both resolution and speed
of analysis. Smaller internal diameters columns (0.25 mm i.d.) can provide
Table 28.2 Selected applications of precip- 3. Fajans titration, which involves the adsorption of a coloured indicator onto
good resolution of early eluting peaks (Fig. 32.14(a)). However, the problem
itation titrations thethat
precipitate at the end-point, resulting in a colour change. During this
Box 4.2 How to interconvert SI units is that the analysis times of the eluting components may be longer and the
linear dynamic Analyte
range may beComments restricted. In contrast, larger internaladsorption
diameter process a change occurs in the indicator resulting in a change
Example: You are required to calculate the molecular 2. Look at the units and decide which are common: columns (0.53 mm i.d.) provide less resolution for early eluting compounds of colour. The indicators used for this are often anionic dyes, e.g. fluores-
weight of a polymer by measurements of its osmotic since the gas constant is expressed in joules, you (Fig. 32.14b), butCl - ,this
Br - is reflected
Mohr in
method: 2CrO4 used
shorterAganalysis cein or lin-
times and a greater eosin. The most common indicator for AgCl is dichlorofluorescein
pressure in solution. At infinite dilution, measured should convert the osmotic pressure term into joules. ear dynamic range. This type as of end-point
column may provide sufficient resolution(Fig. 28.2)
for (this is greenish yellow in solution but changes colour to pink
graphically from your experiments, the equation below The derived unit for pressure is N m -2 and, since the Br - , I - , AsO
the analysis of complex -
mixtures. Fig.
Volhard
4 precipitate the effects when
32.14 illustrates
method: it is adsorbed on AgCl).
of column
applies: derived units for N are J m -1, the full derived unit of removal is unnecessary
internal diameter. Selected examples of precipitation titrations are shown in Table 28.2.
pressure is (J m -1) * m -2 = J m -3.
Π RT Cl - , CN- , Volhard method: precipitate
= CO32- removal is required
c Mr 3. Substitute the units into the equation for M:
256 Instrumental techniques
RTc JK -1
mol -1
* K * kg m -3 Cl - , Br - , I - , Fajans method: titration with
where Π = osmotic pressure at infinite dilution (Pa),
Mr = = = kg mol-1 SCN- Ag+ . Detection with fluorescein,
R = gas constant (J K -1mol-1), T = temperature (K), Π J m -3 dichlorofluorescein and eosin
c = concentration of solution (kg m -3) and Mr = molecular
weight. 4. Substitute the appropriate numerical values into the F- Titration with Th(NO3)4 to
equation for Mr: you know that the units of the cal- produce ThF4. End-point
1. Re-arrange the equation for Mr: M32 Practical Skills in Chemistry 39920.indd
culation will be correct since the molecular weight is
256 detection with alizarin red S 10/05/2017 19:49
the weight of 1 mole of polymer, expressed in kg. Adapted from: Quantitative Chemical Analysis,
RTc
Mr = 4th edn, D.C. Harris, W.H. Freeman, New York
Π
(1995), p. 176.
Temperature
Definitions
The SI unit is the kelvin, K. The degree Celsius scale has units of the same Sources for further study
STP - Standard Temperature and magnitude, °C, but starts at 273.15 K, the melting point of ice at STP. Temper-
Christian, G.D., Dasgupta, P.K. and Schug, K.A. (2014) Chemical Analysis, 6th edn. Prentice Hall, Harlow,
Pressure = 293.15 K and 101325Pa (or ature is similar to time in that the Celsius scale is in widespread use, but note
Analytical Chemistry, 7th edn. John Wiley & Sons Ltd, Essex.
101.325 kPa or 0.101 325 M Pa). that conversions to K may be required for calculations. Note also that you must
Chichester. McPherson, P. (2014) Practical Volumetric Analysis. RSC,
not use the degree sign (°) with K and that this symbol must be in upper case
to avoid confusion with k for kilo; however, you should retain the degree sign Harris, D.C. (2010) Quantitative Chemical Analysis, 8th Cambridge.
with °C to avoid confusion with the coulomb, C. edn. W.H. Freeman Co., New York. Rubinson, J.F. and Rubinson, K.A. (2003) Contemporary
Jander, G., Jahr, K.-F., Schulze, G. and Simon, J. (2009) Volu- Chemical Analysis. Pearson, Harlow, Essex.
Interconversion of SI units metric Analysis, 17th edn. Walter de Gruyter Inc., Germany. Skoog, D.A., West, D.M., Holler, F.J. and Crouch, S.R.
You will find that the use of SI units simplifies mathematical manipulations Mendham, J., Denney, R.C., Barnes, J.D. and Thomas, (2014) Fundamentals of Analytical Chemistry, 9th edn.
and ensures that you obtain the correct units for the parameter being calculated. M.J.K. (2000) Vogel ’s Textbook of Quantitative Brooks Cole, Belmont, CA.
Remember that you must convert all units into the appropriate SI units, e.g.
masses must be expressed as kg, volumes as m3 and concentrations as kg m -3
or mol m -3, etc., and that you may need to use alternatives in derived units
(Table 4.2). The application of these principles is shown in Box 4.2.
Study exercise
Sources for further study 28.1 You are a major manufacturer of fireworks and ‘potassium nitrate’ (4.0124 g) was dissolved
Anon. (2000) The NIST Reference on Constants, Units and Anon. (2014). Measurement units: the SI. Available: you suspect that your bulk supplier of potas- in water and made up to 250.00 mL. This solu-
Uncertainty. Available: http://physics.nist.gov/cuu/units/ www.bipm.org/en/measurement-units/ sium nitrate, a white crystalline solid, has tion (25.00 mL) required silver nitrate solution
index.html Last accessed 05/01/16. been adulterating the potassium nitrate with (10.3 mL; 0.1 M) for equivalence using dichlor-
Last accessed 05/01/16. [Online information includes the SI brochure: The salt to increase his profits. Your analysis of the ofluorescein as indicator. Calculate the % (w/w)
Anon. Measurement units. Available: www.npl.co.uk/ International System of Units (SI), 9th edn (draft).] ‘potassium nitrate’ gave the following results: salt in the ‘potassium nitrate’.
reference/measurement-units/ Blackman, A. and Gahan, L. (2014) Aylward and Findlay’s
Last accessed 05/01/16. SI Chemical Data, 7th edn. John Wiley & Sons Ltd,
Chichester.
44 The investigative approach Classical techniques 213
M04 Practical Skills in Chemistry 39920.indd 44 10/05/2017 15:49 M28 Practical Skills in Chemistry 39920.indd 213 11/05/2017 09:12
Sources for further study – every chapter is Study exercises are included in every chapter to
supported by a section giving printed and electronic reinforce learning with problems and practical exer-
sources for further study. cises.
xiii

For the student
This book aims to provide guidance and support over the spectroscopy), to separation techniques (chromatography
broad range of undergraduate courses, as well as some and electrophoresis), to electrochemistry, use of radioiso-
postgraduate courses, including laboratory classes, project topes and structural techniques (infrared spectroscopy, nu-
work, lectures, tutorials, seminars and examinations, as clear magnetic resonance spectrometry, mass spectrome-
outlined below: try, X-ray diffraction and thermal analysis).
Chapters 1–7 (The investigative approach) Chapters 41–57 (IT, internet and data
Introduce the initial key aspects of all laboratory work. analysis)
Specifically, the essentials of all practical work, health and Cover all aspects of data, from finding useful and relevant
safety aspects (Risk Assessment and COSHH), making information to solving a problem to useful references on
measurements, SI Units and their use, scientific method ‘how to’ perform statistical tests.
and design of experiments, making notes of practical exer-
cises and project work.
Chapters 58–65 (Study and examination
skills)
Chapters 8–12 (Fundamental laboratory
techniques) Focus on the specific skills that will allow you to work ef-
fectively to achieve optimum success during your course
Cover all aspects of laboratory procedures including work-
and beyond.
ing with liquids, solution chemistry and pH and buffer solu-
tions.
Chapters 66–71 (Communicating
Chapters 13–28 (Laboratory techniques) information)
Introduce all the basic laboratory techniques for use Are key to success in chemistry; these chapters provide
in chemistry. Their contents range from basic tech- the essential components that you need to consolidate or
niques used in synthetic chemistry (e.g. melting point, improve upon to succeed.
recrystallisation, solvent extraction, distillation, reflux and
evaporation) through to more advanced areas (e.g. inert Study exercises
atmosphere techniques and combinatorial chemistry). In Provide a valuable resource to allow you to practice and
addition, classical techniques for qualitative inorganic analysis revise key aspects of selected chapters. Answers are
are covered as well as quantitative approaches (including provided at the back of the book. For numerical exercis-
gravimetry, molecular formulae and titrimetry techniques). es, the working out is also provided, as well as the final
answer. In some cases, the answer is in the form of tips
Chapters 29–40 (Instrumental techniques) to allow you to investigate further or provide the direc-
Cover essential relevant analytical instrumental techniques tion for a suitable answer.
from the analysis of molecules (basic spectroscopy), ele- We hope that you find this book a useful resource
mental analysis (atomic spectroscopy, X-ray fluorescence throughout your chosen course, and beyond.
xiv

Acknowledgements
We are grateful to the following for permission to repro- Chemistry; Screenshots 44.4, 44.5 from www.rsc.org/
duce copyright material: merck-index, reproduced with permission from the Royal
Society of Chemistry; Screenshots 44.6, 44.7 from www.
EPSRC funded National Chemical Database Service hosted
chemspider.com, reproduced with permission from the
by the Royal Society of Chemistry; MassBank: a public repos-
Royal Society of Chemistry; Screenshots 44.10, 44.11
itory for sharing mass spectral data for life sciences; North-
from http://www.massbank.jp/, reproduced with permis-
umbria University for the Risk Assessment, COSHH (short)
sion of MassBank Project.
and COSHH (extended) forms; and, Sigma Aldrich Ltd. for
Hazards Statements, Precautionary Statements, Pictograms
– hazard codes and MSDS for phenol (as an example). Tables
While every effort has been made to trace the own- Table 2.1 from http://www.sigmaaldrich.com/help-
ers of copyright material, in a few cases this has proved welcome/hazard-and-precautionary-statements.html,
impossible and we take this opportunity to offer our apol- reproduced with permission from Merck; Table 2.4 from P
ogies to any copyright holders whose rights we may have Statements, http://www.sigmaaldrich.com/help-welcome/
unwittingly infringed. hazard-and-precautionary-statements.html, reproduced
with permission from Merck; Table 44.4 from http://
Figures usefulchem.wikispaces.com/EXP284, McBride, M.J. and
Figure 2.4 from P Statements, http://www.sigmaaldrich. Bradley, J.C., work was completed using Open Notebook
com/help-welcome/hazard-and-precautionary-statements. Science under the supervision of the late Dr. Jean-Claude
html, reproduced with permission from Merck; Figure 2.5 Bradley.
from www.sigmaaldrich.com, reproduced with permis-
sion from Merck; Figure 33.11 from Protein concentration
Picture Credits
by precipitation with pyrogallol red prior to electropho-
resis, Electrophoresis (Marshall, T., Abbott, N.J., Fox, P., The publisher would like to thank the following for their
and Williams, K.M. 1995), Courtesy of Marshall, T. and kind permission to reproduce their photographs:
Williams, K.M., International Electrophoresis Society,
(Key: b-bottom; c-centre; l-left; r-right; t-top)
reproduced with permission of John Wiley & Sons Inc. via
Copyright Clearance Center; Figures 33.13, 33.14 from 123RF.com: Vitaliy Malievsky 240b; John Dean: 175/20.2,
http://www.beckmancoulter.com/products/splashpage/ 240tl/30.21, 247/31.8, 247/31.9, 248/31.13, 248br/31.14,
chiral38/default.asp/, Copyright © 1909–2002, Beckman 272/32.24, 316/35.5; Science Photo Library Ltd: Klaus
Coulter, Inc. Guldbrandsen 274t; Shutterstock.com: Strelch 240bl
/30.22
Screenshots
Screenshots 44.1, 44.2, 44.3 from http://cds.rsc.org, All other images © Pearson Education
reproduced with permission from the Royal Society of

xv

List of abbreviations
A absorbance EOF electroosmotic flow

AAS atomic absorption spectroscopy ESI electrospray ionisation
AC affinity chromatography
ACN acetonitrile F Faraday constant
ACS American Chemical Society FAAS flame atomic absorption spectroscopy
AES atomic emission spectroscopy FID flame ionisation detector
ANOVA analysis of variance FT Fourier transform
AO atomic orbital FT–IR Fourier transform–infrared spectroscopy
APCI atmospheric pressure chemical ionisation GC gas chromatography
Ar relative atomic mass GC–MS gas chromatography–mass spectrometry
ASE accelerated solvent extraction GFC gel filtration chromatography
ATP adenosine triphosphate GPC gel permeation chromatography
ATR Attentuated Total Reflection
h Planck constant
b.pt. boiling point HASAW hazards at work
CCD central composite design HCB hexachloro-1,3-butadiene
CCP cubic close packed HCL hollow cathode lamp
CE capillary electrophoresis HCP hexagonal close packed
CEC capillary electrochromatography HEPES N-(2-hydroxyethyl)-N’-piperazine ethane
CGE capillary gel electrophoresis sulphonic acid
CI chemical ionisation HIC hydrophobic interaction chromatography
COSHH control of substances hazardous to health HPLC high performance liquid chromatography
COSY Correlation Spectroscopy HS headspace
CoV coefficient of variation HRMS high resolution mass spectrum
CRM certified reference material HTML hypertext markup language
CW continuous wave ICP inductively coupled plasma
CZE capillary zone electrophoresis ICP–MS inductively coupled plasma–mass
spectrometry
dp decimal point
IEC ion exchange chromatography
DAD diode array detection
IEF isoelectric focusing
DCM dichloromethane
IR infrared (radiation)
DEPT distortionless enhancement by polarisation
transfer ISE ion selective electrode
DNA deoxyribonucleic acid IUPAC International Union of Pure and Applied
Chemistry
dpm disintegrations per minute
DSC differential scanning colorimetry Ka acid dissociation constant
DTA differential thermal analysis kg kilogram
DVB divinylbenzene Kow octanol–water partition coefficient
Ks solubility product
ECD electron capture detector
Kw ion product of water
EDTA ethylenediaminetetraacetic acid
EI electron impact (ionisation) LC–MS liquid chromatography–mass spectrometry
EIE easily ionisable element LGC Laboratory of the Government Chemist
EF empirical formula LOD limit of detection
EMR electromagnetic radiation LOQ limit of quantitation
en ethylenediamine LRMS low resolution mass spectrum
xvi

List of abbreviations
m.pt. melting point RA relative abundance

MAE microwave assisted extraction Rf relative frontal mobility
MDL minimum detectable level RNA ribonucleic acid
MEKC micellar electrokinetic chromatography RP–HPLC reversed phase high performance liquid
MEL maximum exposure limit chromatography
MF molecular formula rpm revolutions per minute
MO molecular orbital RSC Royal Society of Chemistry
Mr relative molecular mass RSD relative standard deviation
MS mass spectrometry SAX strong anion exchange
NH null hypothesis SCOT support coated open tubular (column)
NIST National Institute of Standards and SCX strong cation exchange
Technology SDS sodium dodecyl sulphate
NMR nuclear magnetic resonance SE standard error (of the sample mean)
NP–HPLC normal phase high performance liquid SEM scanning electron microscopy
chromatography SFE supercritical fluid extraction
SI Système Internationale D’Unités
ODS octadecylsilane SPE solid phase extraction
OEL occupational exposure standard SPME solid phase microextraction
PAGE polyacrylamide gel electrophoresis STP standard temperature and pressure
PCA principal component analysis TCA trichloroacetic acid
pdf portable document format TCD thermal conductivity detector
PDMS polydimethylsiloxane TG thermogravimetry
PEEK poly(etheretherketone) TLC thin layer chromatography
PFA perfluoroalkoxyvinylether TMS tetramethylsilane
PFA perfluoroalkoxy fluorocarbon TOF-MS time-of-flight mass spectrometry
PFE pressurised fluid extraction TRIS tris(hydroxymethyl)aminomethane or
pH log10 proton concentration (activity) 2-amino-2-hydroxymethyl-1,3-propanediol
PLOT porous layer open tubular (column)
UKAS United Kingdom Accreditation Services
PMT photomultiplier tube
URL uniform resource locator
ppb parts per billion (109)
USEPA United States Environmental Protection
PPE personal protection equipment Agency
ppm parts per million (106) UV ultraviolet
PTFE polytetrafluoroethylene
WCOT wall-coated open tubular (column)
QA quality assurance www World Wide Web
R universal gas constant z net charge on an ion
xvii

The investigative approach
1. Essentials of practical work 3
2. Health and safety 6
3. Making measurements 36
4. SI units and their use 40
5. Scientific method and design of experiments 46
6. Making notes of practical work 52
7. Project work 56

1 Essentials of practical work
All knowledge and theory in science has originated from practical observation
Developing practical skills – these will
and experimentation: this is equally true for chemical disciplines as diverse as
include:
analysis and synthesis. Laboratory work is an essential part of all chemistry
●● designing experiments
●● observing and measuring
courses and often accounts for a significant proportion of the assessment marks.
●● recording data
The skills and abilities developed in practical classes will continue to be useful
●● analysing and interpreting data throughout your course and beyond, some within science and others in any
●● reporting/presenting. career you choose (see Chapter 58).
Being prepared
Safety Note Mobile phones –
these should never be used in a lab Key Point You will get the most out of laboratory work if you
class, as there is a risk of contamination prepare well. Do not go into a practical session assuming that
from hazardous substances. Always everything will be provided, without any input on your part.
switch off your mobile phone before
entering a laboratory. The main points to remember are:
●● Read any handouts in advance: make sure you understand the purpose
of the practical and the particular skills involved. Does the practical relate
to, or expand upon, a current topic in your lectures? Is there any additional
preparatory reading that will help?
Using textbooks in the lab – take this

●● Take along appropriate textbooks, to explain aspects in the practical.
book (or photocopies of relevant pages) ●● Consider what safety hazards might be involved, and any precautions
along to the relevant classes, so that you might need to take, before you begin (p. 6).
you can make full use of the informa-
tion during the practical sessions.
●● Listen carefully to any introductory guidance and note any important
points: adjust your schedule/handout, as necessary.
●● During the practical session, organise your bench space – make sure your
lab book is adjacent to, but not within, your working area. You will often find
it easiest to keep clean items of glassware, etc., on one side of your working
Safety Note If in doubt over any space, with used equipment on the other side.
part of the practical procedure – ASK!
There is no such thing as a silly ques-
●● All chemical waste (solid or liquid) should be disposed of in the
tion in the laboratory.
appropriate containers provided (consult the demonstrator or lecturer-
in-charge).
●● Write up your work as soon as possible and submit it on time or you may
lose marks.
●● Catch up on any work you have missed as soon as possible – preferably
before the next practical session.
Basic requirements
Presenting results – while you don’t Recording practical results
need to be a graphic designer to pro-
duce work of a satisfactory standard,
An A4 loose-leaf ring binder offers flexibility, since you can insert laboratory
presentation and layout are important
handouts, and lined and graph paper, at appropriate points. The danger of losing
and you will lose marks for poorly pre-
one or more pages from a loose-leaf system is the main drawback. Bound books
sented work.
avoid this problem, although those containing alternating lined/graph or lined/
blank pages tend to be wasteful – it is often better to paste sheets of graph paper
into a bound book, as required.

Essentials of practical work
All experimental observations and data should be recorded in a notebook

Presenting results – layout and pres-
in ink at the time they are made because it is easy to forget when you are busy.
entation of work are important. Ensure
A good-quality HB pencil or propelling pencil is recommended for making
that the information presented is legi-
diagrams, etc. as mistakes are easily corrected with a vinyl eraser. Buy a black,
ble. You will lose marks for poorly pre-
spirit-based (permanent) marker to label experimental glassware, sample tubes,
sented work. Chapter 6 gives further
etc. Fibre-tipped fine line drawing/lettering pens are useful for preparing final
practical advice.
versions of graphs and diagrams for assessment purposes. Use a clear ruler
(with an undamaged edge) for graph drawing, so that you can see data points/
information below the ruler as you draw.
Using calculators for numerical Calculators

problems – Chapter 6 gives further These range from basic machines with no pre-programmed functions and only
advice. one memory, to sophisticated programmable minicomputers with many mem-
ories. Note: Many university departments specify a particular make and model
of calculator for use in examinations. It is important that you purchase and
become familiar with the use of this calculator. The following may be helpful
when using a calculator:
●● Power sources. Choose a battery-powered machine, rather than a mains-
operated or solar-powered type. You will need one with basic mathematical/
scientific operations including powers, logarithms (p. 472), roots and paren-
Using calculators – take particular care theses (brackets), together with statistical functions such as sample means
when using the exponential key ‘EXP’ and standard deviations (Chapter 53).
or ‘EE’. Pressing this key produces
10 something. For example, if you want
●● Mode of operation. Calculators fall into two distinct groups. The older
to enter 2 * 10 -4 , the order entry is 2,
system used by, for example, Hewlett Packard calculators is known as the
EXP, - , 4 not 2, * , 10, EXP, - , 4.
reverse Polish notation: to calculate the sum of two numbers, the sequence
is 2 [enter] 4 + and the answer 6 is displayed. The more usual method of
calculating this equation is as 2 + 4 =, which is the system used by the
majority of modern calculators. Most newcomers find the latter approach
Using inexpensive calculators – many to be more straightforward. Spend some time finding out how a calculator
unsophisticated calculators have a operates, e.g. does it have true algebraic logic (U then number, rather than
restricted display for exponential num- number then U)? How does it deal with scientific notation (p. 471)?
bers and do not show the ‘power of 10’,
e.g. displaying 2.4 * 10-5 as 2.4-05, or
●● Display. Some calculators will display an entire mathematical operation
2.4E–05, or even 2.4–05.
(e.g. ‘2 + 4 = 6 ’), while others simply display the last number/operation.
The former type may offer advantages in tracing errors.
●● Complexity. In the early stages, it is usually better to avoid the more com-
plex machines, full of impressive-looking, but often unused preprogrammed
functions – go for more memory, parentheses or statistical functions rather
than engineering or mathematical constants. Programmable calculators may
be worth considering for more advanced studies. However, it is important to
note that such calculators are often unacceptable for exams.
Presenting more advanced practical work

In some practical reports and in project work, you may need to use more
sophisticated presentation equipment. Word processing may be essential and
Presenting graphs and diagrams –
computer-based graphics packages can be useful. Choose easily read fonts
ensure these are large enough to be
such as Arial or Times New Roman for project work and posters and consider
easily read: a common error is to pres-
the layout and content carefully (p. 601). Alternatively, you could use fine line
ent graphs or diagrams that are too
drawing pens plus dry-transfer lettering and symbols, such as those made by
small, with poorly chosen scales (see
Letraset®, although this approach is usually more time consuming and less
p. 453).
flexible than computer-based system, e.g. using Microsoft Excel.
4 The investigative approach

Essentials of practical work
The use of Microsoft PowerPoint® as a presentation package is common

Printing on acetates – standard over-
place. It is common to find a computer and presenter available for student use.
head transparencies are not suitable for
Advice on content and presentation is given in Chapter 68.
use in laser printers or photocopiers:
you need to make sure that you use the
correct type.
Source for further study

Bennett, S.W. and O’Neale, K. (1999) Progressive Devel- Overton, T., Johnson, S. and Scott, J. (2015) Study and
opment of Practical Skills in Chemistry. A guide to Communication Skills for the Chemical Sciences,
early-undergraduate experimental work. Royal Society 2nd edn., Oxford University Press, Oxford.
of Chemistry, Cambridge.
Study exercises
1.1 Consider the value of practical work. Spend a few 1.3 Check your calculator skills. Carry out the fol-
minutes thinking about the purpose of practical lowing mathematical operations, using either
work within a specific part of your course (e.g. a a hand-held calculator or a PC with appropriate
particular first year module) and then write a list of ‘calculator’ software.
the six most important points. Compare your list
(a) 5 * (2 + 6)
with the generic list we have provided on p. 602,
(b) [8.3 , (6.4 - 1.9)] * 24 (to 4 significant
which is based on our experience as lecturers –
figures)
does it differ much from your list, which is drawn
(c) (1 , 32) * (5 , 8) (to 3 significant figures)
up from a student perspective?
(d) 1.2 * 10 5 + 4.0 * 10 4 in scientific notation
1.2 Make a list of items required for a particular prac- (see p. 471)
tical experiment. This exercise is likely to be most (e) 3.4 * 10 -2 - 2.7 * 10 -3 in ‘normal’ notation
useful if you can relate it to an appropriate prac- (i.e. conventional notation, not scientific for-
tical session on your course. However, we have mat) and to 3 decimal places.
given a model list for a recrystallisation of an
impure compound from water as an example. (See also numerical exercises in Chapter 51)

2 Health and safety
Health and safety law requires institutions to provide a working environment

Health and Safety Legislation – in the
that is safe and without risk to health. Where appropriate, training and informa-
UK, the Health and Safety at Work Act
tion on safe working practices must be provided. Students and staff must take
1974 provides the main legal framework
reasonable care to ensure the health and safety of themselves and of others, and
for health and safety.The Control of Sub-
must not misuse any safety equipment.
stances Hazardous to Health (COSHH)
Regulations 2002 impose specific legal
requirements for risk assessment wher- Key Point All practical work must be carried out with safety
ever hazardous chemicals or biological in mind, to minimise the risk of harm to yourself and to others –
agents are used, with Approved Codes safety is everyone’s responsibility by law.
of Practice for the control of hazardous
substances, carcinogens and biological
agents, including pathogenic microbes. Risk assessment
A risk assessment is a systematic approach to hazard identification and control.
It is essential to consider what aspects of a laboratory activity can cause injury
to people and then to introduce control measures that will reduce the risk of
injury to an acceptable level. Important aspects to consider are:
●● Substance hazards
●● How the substance is to be used
Definitions
●● How it can be controlled
Hazard – the potential of a substance to
cause harm. ●● Who is exposed
Risk – the likelihood that a substance ●● How much exposure
will harm you and the severity of harm
in the actual circumstances of use. ●● The duration of exposure
Key Point It is important to distinguish between the HAZARD

of a substance and the RISK resulting from exposure.
The risk assessment process

The five step process requires you to:
1. Identify the hazards and risk: One way to do this is by using ‘PEME,’
i.e. People, Equipment, Materials and Environment.
a. ‘People’ hazards can cover a range of issues including the individual
themselves and the systems that people have to use. In this ‘people’
context consider the following terms: training, capabilities /restrictions,
supervision, communication, adequate numbers and human error.
b. ‘Equipment’ hazards relate to the equipment to be used; it will also
consider related aspects of the equipment including repair, mainte-
nance, handling, storage, cleaning and operation of the equipment.
c. ‘Materials’ hazards cover any liquid, solid or gas associated with
the task. This aspect also covers any by-products or waste generated
by the activity.

Health and safety
splash d. ‘Environment’ hazards relate to the surrounds you are working in.
inhalation
Examples include poor lighting, heating and ventilation, poor access
and egress, tripping/slipping hazards, restricted space/visibility and
ingestion
other activities taking place nearby.
2. Identify who can be harmed and how: Who – Athough a task may
intravenous
or seem to be well managed, if control measures fail then a whole range of
absorption people could be injured, e.g. co-lab workers in the area or people visiting
the area. Your risk assessment should consider all those people who could
potentially be harmed if the control measures fail. How – the five routes of
chemical exposure (Fig. 2.1) are: inhalation – breathing in small particles
or chemical vapours is the most common exposure pathway; dermal –
some chemicals can be absorbed into the body; ingestion – inadvertent
absorption
hand-to-mouth transmission; intravenously – improper use of needles/
(dermal) from glass pipettes and their disposal can lead to inadvertent exposure; eye
spillage contact – rubbing your eyes after chemical exposure with your hands (with
or without gloves).
Fig. 2.1 Major routes of entry of harmful 3. Identify the current controls and decide if more is required
substances into the body. a. Identify the control measures currently in place for each hazard
you have identified i.e. physical controls (i.e. local exhaust ventila-
tion); procedural controls (i.e. a safe working procedure for the task);
and behavioural controls (i.e. adequate supervision and monitoring of
Safety Note behaviour).
Protective clothing is worn as a first b. Identify the risks and decide on precautions – a risk matrix anal-
barrier to spillage of chemicals on to ysis. A risk analysis is a qualitative estimate of risk associated with
your body. each applicable risk; it assumes that the planned or existing controls
Lab coats are for protection of you and are in place. Box 2.1 shows you how to undertake a risk matrix anal-
your clothing. ysis. The risk matrix evaluates the risk by allocating a numeric risk
Eye protection special spectacles with level and the tolerability of the hazard.
side pieces to protect you from your
own mistakes and those of your col- 4. Record your findings – you will need to record your assessments. You
leagues. If you wear spectacles, eye will need to:
protection with prescription lenses a. state clearly what task /activity the risk assessment covers
and side pieces is available from your
optician, an expensive but worthwhile b. ensure that the hazards and controls are clearly listed
investment. Otherwise goggles can be
worn over spectacles. c. consider all those people who could potentially be harmed
Contact lenses should not be worn in d. ensure that the appropriate member of staff signs off the assessment
the laboratory. Chemicals can get under (e.g. technical demonstrator; lecturer-in-charge; project supervisor)
the lens and damage the eye before the
lens can be removed. It is often very dif- e. make sure the completed risk assessments are readily available to
ficult to remove the contact lens from those who might need them (e.g. module tutor).
the eye after a chemical splash.
5. Review as necessary. Risk assessments should be reviewed on a regular
Shoes should cover the feet: no open-
basis. The period of review should reflect the hazards: the greater the
toed sandals, for example.
hazards the more frequent the review. The risk assessments should also be
Long hair should be tied back and hats
reviewed, if for example, the experiment is modified in any way.
(e.g. baseball caps) should not be worn.

Health and safety
Box 2.1 How to perform a risk matrix analysis
A risk matrix analysis allows you to prioritise the likeli- environment / manner it is used in; in the absence of
hood and severity of risk to an individual from the hazard any specific control measures you should indicate the
identified. highest likelihood among the various risks (Table 2.3).
1. Using the form in Fig. 2.2 conduct a COSHH assess- 5. Assess the ‘severity’; this should be substance-spe-
ment of the chemical to be used in a practical labo- cific rather than activity-specific. This should relate
ratory class. If the Signal word is DANGER then the directly to the information provided on the MSDS
extended COSHH form should be used (Fig. 2.3). sheet (provided by the manufacturer); use the high-
est severity assessment among the various risks
2. First consult the Material Safety Data Sheet (MSDS) (Table 2.3).
supplied; all manufacturers of hazardous chemicals
are required to provide one of these sheets for all 6. Then, calculate the risk rating using the risk matrix
products which they sell. (Table 2.4). The risk is calculated by multiplying the
likelihood by the severity before any control meas-
3. Consult the Hazard pictograms (Fig. 2.4) for visible ures additional to Good Laboratory Practice (GLP)
relevant information. In addition, H (hazard) state- / Personal Protective Equipment (PPE) – laboratory
ments (Table 2.1) and P (precautionary) statements coat and safety glasses are factored in. This calcula-
(Table 2.2) are available on MSDS sheets and /or tion of risk should quote the highest risk associated
at: http://www.sigmaaldrich.com/help-welcome/ with the substance (i.e. what is the most dangerous
hazard-and-precautionary-statements.html. Enter feature of the substance).
the compound name in the search facility, then click
‘MSDS’ at the appropriate product line. 7. You are aiming to reduce the likelihood to as close to
1 as you can get (e.g. by performing the experiment
4. Assess the ‘likelihood’ of harm coming to pass in a fume cupboard).
given the amount/nature of substance used, the
An example MSDS sheet for phenol is shown in Fig. 2.5. In addition, an exam-
ple of a completed COSHH form for phenol is shown in Fig. 2.6. In addition,
as the Signal word is Danger an extended COSHH form (Fig. 2.3) would be
All manufacturers of hazardous chem-
required to be completed.
icals are required to provide a Material
Safety Data Sheet, or MSDS. The MSDS
Hazard statements – There are 72 individual and 17 combined Hazard state-
will contain the following information:
ments (Table 2.1). Each one of them is assigned a unique alphanumerical code
●● Manufacturer which consists of one letter and three numbers as follows:
●● Name of Chemical
●● Chemical Components ●● the letter ‘H’ (for ‘hazard statement’);
●● Hazards Associated with the Product ●● a number designating the type of hazard: ‘2’ for physical hazards; ‘3’ for
●● First Aid Measures
health hazards; and ‘4’ for environmental hazards; and finally,
●● Fire Fighting Measures
●● Handling and Storage ●● two numbers corresponding to the sequential numbering of hazards aris-
●● Accidental Release Procedures ing from the intrinsic properties of the substance or mixture, i.e. explosive
●● Exposure Control and Personal properties (codes from 200 to 210), flammability (codes from 220 to
Protection
230), etc.
●● Physical and Chemical Properties
●● Stability and Reactivity
●● Toxicological and Ecological Precautionary statements – There are 116 individual and 33 combined Pre-
Information cautionary statements (Table 2.2). These are assigned a unique alphanumerical
●● Disposal Practices code which consists of one letter and three numbers as follows:
●● Other miscellaneous information
●● the letter “P” (for ‘precautionary statement’);

Health and safety
●● one number designating the type of precautionary statement: ‘1’ for gen-
eral precautionary statements; ‘2’ for prevention precautionary statements;
‘3’ for response precautionary statements; ‘4’ for storage precautionary
statements; and, ‘5’ for disposal precautionary statements; and finally
●● two numbers (corresponding to the sequential numbering of precaution-
ary statements).
Fig. 2.2 Control of Substances Hazardous to Health (COSHH) form

Health and safety
Fig. 2.3 Extended Control of Substances Hazardous to Health (COSHH) form

Another random document with
no related content on Scribd:
En sortant du Campo Santo, nous vîmes s’avancer, marchant en
bon ordre, de longues files d’hommes habillés de gris. Je pensai à
des équipes de forçats commandés pour la corvée des routes. Ils
portaient des blouses de toile et des pantalons rapiécés, de
grossières espadrilles laissant voir leurs pieds nus, et ils étaient
coiffés de méchants bonnets de police. Un coup de clairon m’apprit
que j’avais en face de moi la troupe. C’étaient, en effet, deux
compagnies d’infanterie garnisonnées à Estella qui partaient pour la
manœuvre. On les accoutre ainsi par économie, afin de ménager la
tenue de drap réservée pour les grandes occasions. Pauvreté n’est
pas vice, et l’économie est une belle chose, mais je doute que des
fantassins ainsi affublés se sentent fiers d’être soldats.
Je recommande ce costume à nos niveleurs économes qui
réclament à grands cris l’unification de l’uniforme militaire, ainsi
qu’aux intelligents champions de la suppression des armées
permanentes ; ils ne pourront mieux dégoûter la jeunesse du métier
de Mars. Le nec plus ultra du misérable et du bon marché sera d’un
seul coup atteint.
L’aspect de ces fantassins, petits et grêles, ne rappelle guère
cette redoutable infanterie espagnole « dont les gros bataillons
serrés, dit Bossuet, semblables à autant de tours, mais à des tours
qui sauraient réparer leurs brèches, demeuraient inébranlables au
milieu de tout le reste en déroute… » Certes, je ne mets pas un seul
instant en doute leur énergie et leur vaillance, je ne parle que de
l’extérieur, et il ne paye pas de mine. Il est vrai que leur uniforme, qui
semble une copie maladroite du nôtre, n’est pas de nature à la
rehausser. A Gibraltar surtout, à côté des superbes et corrects
soldats anglais, cette apparence défectueuse d’une armée mal
accoutrée, mal payée et mal nourrie, frappe l’œil désintéressé de
l’étranger.
C’est à Estella que je fus, pour la première fois, réveillé en
sursaut par une voix lamentable. Elle jetait par intervalles, des
profondeurs d’une rue voisine, des modulations prolongées et
lugubres qui approchaient grandissant, éclataient sous mes fenêtres,
puis s’éloignaient et retournaient se perdre dans la nuit.
Ce sont les serenos, gardes de nuit, qui crient le temps et l’heure
en commençant par une invocation à la Vierge : « Ave Maria
sanctissima ! Il est minuit. Le temps est serein ! » Ce chant nocturne,
car il est rythmé comme tous les cris de rue, restant de vieilles
coutumes générales dans presque toute l’Europe, ne manque pas
d’originalité. L’usage, il n’y a pas longtemps encore, existait chez
nous dans nombre de villes de province. A Douai, il y a dix ou quinze
ans, un homme criait les heures au beffroi. Mais c’est surtout au
siècle dernier que le veilleur de nuit offrait un aspect fantastique.
Vêtu d’une longue robe brune, bigarrée de têtes de mort et de tibias
en sautoir, il passait à pas lents, agitant une cloche et criant d’une
voix sépulcrale :
Réveillez-vous, gens qui dormez,

Priez pour les trépassés.
Les serenos, à Madrid, ouvrent la porte aux locataires attardés.

Chaque quartier, chaque rue, a les siens ; ils ont les clefs de toutes
les maisons. On se passe ainsi de concierge, et les bourgeois
peuvent dormir sur leurs deux oreilles :
Car sur la grande ville

Veille un brave gardien,
C’est le bon mile, mile,
C’est le bon milicien !
X
LOGROÑO
Depuis notre entrée en Espagne, nous avons traversé de

merveilleux paysages, d’abord en côtoyant le golfe, puis, à mesure
que nous nous enfoncions par les chemins de la montagne, le
panorama se déroulait pittoresque, varié ; villages enfouis dans des
nids de verdure, bourgades échelonnées sur les flancs d’un mont,
vieux ponts croulants jetés sur des abîmes.
Mais passé Estella, la scène n’est plus la même, l’aspect du pays
change presque subitement ; la végétation diminue ; de grandes
roches à aiguille se dressent çà et là au milieu de bouquets de
chênes qui vont en s’éclaircissant.
Après la Navarre, nous entrons dans la vieille Castille. Ce sont
des montagnes arides, des bourgades qu’on aperçoit tout à coup
comme des forteresses arabes au sommet d’un pic, sans un arbre,
sans un brin de verdure, le pays brûlé. Mais dans une trouée, une
crevasse du roc, au fond d’un vallon reparaît tout à coup la
luxuriante flore des chaudes régions, vignes, figuiers, oliviers. Il
semble que le sol séché et grisâtre ait craqué, laissant de longues
déchirures où la végétation s’entasse comme si la nature féconde
voulait se dédommager de la stérilité d’alentour. D’Estella à Logroño,
la route large et soutenue par des travaux de maçonnerie a dû
coûter gros, vu les accidents de terrain. L’Espagne est sillonnée de
ces belles routes ne servant guère et se détériorant de distance en
distance par morceaux qui s’effritent et s’écroulent. Les Espagnols
qui voyagent soit à pied — et ils sont rares — soit à cheval ou à
mule, prennent autant que possible les chemins de traverse. C’est
ce que nous faisions généralement, laissant la voie royale aux
piétons sybarites qui craignent de s’échauffer par les sentiers
raboteux. Reste la diligence qui s’arrange comme elle peut. Quant
aux cantonniers, ils en prennent à leur aise et travaillent à leurs
heures. « Le cantonnier en Espagne, disait plaisamment le vieux
Dumas, voyageur fantaisiste, est un individu qui a pour mission,
drapé dans un grand manteau amadou, de regarder passer les
gens. » Le fait est qu’ils ont chacun trois kilomètres à entretenir, en
plein soleil, travail terrible pour un Espagnol. De six kilomètres en six
kilomètres, on leur a bâti de petites maisons pour deux familles.
Dans les grandes plaines désolées de la Manche, dans les gorges
profondes des Sierras, je me suis demandé bien souvent ce que
pouvait faire la femme livrée à la solitude tout le jour. Il est vrai qu’il y
a la marmaille, graine absorbante, les visites des bergers du
voisinage, le passage des coches et des muletiers. Quelques-unes
vendent en cachette, car l’administration le leur défend, de
l’aguardiente à un sou le verre ; maigre ressource, le débit d’une
bouteille est une affaire qui demande du temps.
Nous en avons rencontré une dans la Sierra Morena qui nous
offrit l’hospitalité : bon feu et gîte passable ; quant au reste… le mari
le saisit. C’était une belle luronne de vingt-cinq à vingt-six ans, brune
à souhait, aux seins dodus, méritant mieux que l’incessant
tripotement d’un affreux marmot qui semblait payé pour les
déformer. Elle baragouinait un peu de français, et nous raconta au
souper, non entre la poire et le fromage — le luxe du dessert n’ayant
pas encore pénétré dans la Sierra — mais entre la soupe à l’huile
alliacée et le vin goudronné, qu’elle avait été jadis servante dans une
fonda de Logroño, et qu’un caballero français des mieux tournés lui
avait proposé de l’emmener là-bas, là-bas, tra los montes. Elle
faisait de grands gestes avec la main pour indiquer que la France
était à ses yeux si éloignée, qu’elle se perdait dans l’espace. Le
cantonnier écoutait d’un air admiratif le jargon pour lui
incompréhensible de son épouse tout en fumant philosophiquement
sa cigarette.
Nous demandâmes à la jeune femme s’il était jaloux. Elle leva les
yeux au ciel avec un geste expressif.
Il a chassé malhonnêtement le padre du village voisin parce que
le saint homme venait ici en son absence.
Sur la poitrine velue du mari s’étalent cependant un scapulaire
fort crasseux et deux ou trois médailles de cuivre usées, indice d’un
long usage, et qui eussent dû témoigner de plus de confiance de sa
part. Mais, en Espagne, catholicisme n’implique pas cléricalisme. En
nombre de provinces, on est froid pour le prêtre tout en fanatisant
chaudement au pied de l’autel ; on ferme sa porte à l’apôtre, d’autant
plus qu’on a jolie femme, mais on écoute dévotement le sermon.
L’abolition des dîmes, le désamortissement des biens du clergé,
la suppression des couvents, la sécularisation de l’enseignement ont
été partout accueillis avec enthousiasme, et cependant pas de
peuple ne s’agenouille avec plus de foi devant les images et
n’invoque avec plus de ferveur la Virgen Santissima, ne baise plus
dévotement ses chapelets et ses agnus.
Logroño est une ville de quinze à vingt mille âmes, avec une
garnison qui m’a paru nombreuse ; elle n’offre de curieux que ses
églises et quelques vieilles rues. Nous avions une lettre
d’introduction pour le gouverneur, appelé ici brigadier général. Il ne
nous fut donné de voir que son premier aide de camp, que nous
rencontrâmes sur une promenade assez sèche et poudreuse
appelée las Delicias, où lui seul, superbe garçon, semblait faire en
effet les délices d’un groupe animé de jeunes señoritas.
Après l’absorption de consommations à la glace — pour la
confection desquelles les limonadiers espagnols n’ont pas de rivaux
— nous gagnâmes le comedor, où nous trouvâmes la banalité
commune à tous les hôtels.
Seulement, pas de garçon. De jolies filles fort dégourdies les
remplaçaient avantageusement.
De la salle à manger j’aperçois les deux étranges flèches
guillochées de l’église de Santiago, où se fonda, dit-on, l’ordre de
chevalerie de ce nom. De gros nids de cigognes sont accrochés à
chacune des aiguilles et, perchées sur le bord, elles claquent
mélancoliquement du bec. En bas, dans la rue étroite, monte le
chant doux et un peu traînard de jeunes filles qu’accompagne un
tambour de basque, musique bientôt couverte par les aigres
disputes des servantes de l’hôtel qui, avec la verbosité méridionale,
s’apostrophent abominablement au sujet d’une carafe cassée.
Après dîner, le hasard me pousse dans une antique petite église
d’extérieur assez misérable ; mais quel luxe au dedans ! Luxe de
vieux tableaux surtout ; l’un presque dissimulé dans un coin sombre
attira spécialement mon attention. Il représentait une sainte à robe
montante jusqu’au menton, avec un voile couvrant le front et les
épaules, ne laissant à découvert que les mains et le visage, mais
dans un drapement si savamment voluptueux qu’il valait toutes les
splendeurs du nu. C’est Rose de Lima. Agenouillée, bras en croix,
corps en arrière, dans l’extase, elle semble jouir par avance de
célestes béatitudes. Et il y a de quoi, car un beau séraphin accourt
impatient, perçant les nues pour lui apporter une couronne de roses.
Sur le divin corps de la sainte pâmée, l’artiste a collé, comme une
draperie mouillée, sa robe de dominicaine, dessinant avec une telle
exactitude les provocantes ampleurs des hanches et les contours du
ventre et des seins que, dans la pénombre, elle semblait
entièrement nue. Un voile sombre comme une chevelure noire
couvrant ses épaules jusqu’à ses rotondités postérieures complète
l’illusion. Jamais lascive abbesse posant pour la chaste Suzanne
aux yeux ravis de quelque Rubens monacal ne fut plus
scrupuleusement et plus amoureusement peinte. Le visage, surtout,
est remarquable d’ardente passion. En s’approchant, on distingue de
petites touffes crépelées d’un blond vénitien s’échappant de chaque
côté du voile, près de la mignonne oreille. Il était visible que la belle
créature avait exigé de l’artiste admirateur ce sacrifice à la sincérité
du costume pour paraître plus séduisante. L’œil bleu foncé se noyait
dans la jouissance extatique ; la bouche entr’ouverte aux lèvres
sensuelles humait des plaisirs inconnus aux humains.
« Eh bien, voilà comme j’aime les saintes ! » m’exclamai-je in
petto, pour ne pas profaner le lieu sacré.
Le vieux sacripant de bedeau qui m’examinait, lut sans doute ma
pensée dans mon œil.
« Ah ! dit-il en soupirant, on n’en fait plus dans ce goût-là. »
XI
LE COL DE PIQUERAS
Il n’est pas de vrai voyage en Espagne sans histoire de

brigands ; j’y comptais, et si je n’avais pas eu mon histoire de
brigands, je considérerais mon excursion manquée. Dans un pays
où l’on arrête encore non seulement les coches — ce qui est
l’enfance de l’art — mais les trains de chemin de fer, deux touristes
pérégrinant, sac au dos, doivent s’attendre à quelque aventure
cartouchienne ; aussi en étions-nous à peine à notre quinzième
journée de marche, après avoir couché à Villanueva de Cameros et
traversé l’Iregua, que nous fûmes pris dans une venta isolée de ce
malaise qui saisit, dit-on, les plus braves lorsqu’on sent des dangers
inconnus rôder comme des loups dans les affres de la nuit.
En pleine Sierra de Cebollera, près du point culminant qui sépare
les provinces de Soria et de Logroño, nous arriva cette mémorable
aventure. L’endroit est propice aux choses tragiques, désert et
suffisamment sauvage. Il y vente sans cesse et il y souffle même
dans les matinées d’été un froid de loup. Aussi les loups semblent y
avoir établi leur quartier général.
Des forêts de hêtres qui couvrent les hauteurs leur offrent dans
l’été un refuge assuré, et les troupeaux qui paissent dans les
pâturages des flancs des monts et des creux des vallons, une assez
suffisante pitance. J’ai ouï dire que la bourgade de Lumbreras, au
milieu de la Sierra de Cameros, à quelques kilomètres de celle de
Cebollera, possédait autrefois quatre-vingt mille moutons, réduits
aujourd’hui à trois mille. Les bonnes gens de la montagne
prétendent que la différence est passée dans le ventre des loups. Je
suppose qu’on exagère et que l’épizootie et l’incurie castillane ont
été plus funestes aux moutons que le terrible appétit des
carnassiers.
Quoi qu’il en soit, bien avant la venue d’octobre, la neige couvre
déjà les sierras, et pendant plusieurs mois, le pays entier est bloqué.
Gens et bêtes hivernent dans les fermes avec les provisions d’une
place assiégée. Alors les loups affamés descendent. Par bandes de
dix à vingt ils entourent les habitations isolées, hurlant jusqu’au jour
aux portes des étables le lamentable cri de la famine. Ces pauvres
bêtes ont, comme tout le monde, un estomac à satisfaire, et, comme
les anarchistes, réclament le droit au gigot. Moutons, vaches,
chevaux, chiens, enfants, tout ce qui tombe sous leur dent y passe,
et au matin ils regagnent lentement la forêt. On en détruit bien un
grand nombre, mais ça repousse. Puis, à quoi bon ? leur peau ne
vaut pas le coup de fusil, et autant que l’Arabe, l’Espagnol est
ménager de sa poudre. On les laisse donc pulluler, comptant que la
misère et la faim les tueront comme elles tuent les races trop
prolifiques, et que, comme les races trop prolifiques aussi, les loups,
à l’encontre du proverbe, finiront par se manger entre eux.
La venta de Piqueras forme le point central de ces territoires
misérables. C’est un long bâtiment délabré, très bas, sans fenêtre au
rez-de-chaussée, avec un seul étage. Deux portes cochères y
donnent accès, mais l’une est celle d’une chapelle dont le clocheton
se dresse à l’extrémité du toit. C’est là que nous heurtâmes, après
avoir vainement frappé à la première. Elle était ouverte et nous nous
trouvâmes dans un sanctuaire du genre de celui du palacio
d’Urvaza, aspect réjouissant pour de pieux pèlerins, mais lamentable
pour des profanes affamés.
Nous appelons : « Hé ! le maître ? Hé ! le curé ? Hé ! le
sacristain ? » rien. Nous retournons à la porte première que nous
secouons à grands coups de pied.
A quelque distance, un homme et deux petites filles battaient le
blé à la manière arabe, c’est-à-dire à l’aide d’un cheval, qui en
tournant écrase les gerbes. Ils nous voyaient bien heurter, mais
continuaient leur besogne sans mot dire.
Nous les hélons.
« Il n’y a personne, nous crie l’homme.
— Où est le maître de la venta ?
— Il ne rentrera qu’à la nuit. »
Nous nous approchons du batteur, qui nous engage comme avait
fait le châtelain d’Urvaza à continuer vivement notre route pour
atteindre la Poveda, village sur le versant opposé, c’est-à-dire à
quatre ou cinq lieues. Mais nous commençons à nous habituer à
l’hospitalité espagnole ; aussi, déposant nos sacs, nous nous
allongeons sur la paille hachée, résolus à attendre le propriétaire de
la venta, dût-il ne rentrer qu’à minuit ; ce que voyant, l’homme dit
quelques mots à l’aînée des petites filles, gamine fort sérieuse, de
dix à onze ans, occupée à balayer le terrain et à mettre en tas le blé
battu.
Elle ramasse une grosse clef, cachée sous la veste paternelle,
appelle sa sœur et nous crie : « Venez, hommes. »
Nous la suivons à la venta, nous traversons une grande étable
vide et entrons dans une cuisine qui d’abord nous parut aussi noire
qu’un four ; et, en effet, elle ne reçoit le jour que par le trou de la
cheminée, percé juste au milieu de la pièce, comme dans les huttes
des Peaux-Rouges. On peut, ainsi qu’à un feu de bivouac, entourer
le foyer et la marmite. Le feu, la cadette le prépare et l’allume, et la
marmite, l’aînée en entreprend le nettoyage avec un bouchon de
paille ; puis elle sort et rentre bientôt avec une énorme cruche pleine
d’eau qu’elle porte sur une de ses hanches.
Étendus sur des bancs, nous goûtions le doux farniente après la
fatigue, et mon regard allait de la flamme joyeuse aux recoins
obscurs de l’antre enfumé où la lumière dansante envoyait ses
reflets, éclairant tout à coup, pour les rejeter dans l’ombre, des
rangées de pots et de vieilles assiettes dressées sur un buffet
rustique ; des casseroles de cuivre, une image de la Vierge, des
guirlandes d’oignons et d’ail, un portrait en pied de torero dont
l’enluminure primitive disparaissait sous une couche de suie, un
morceau de lard jauni accroché à la voûte, un vase à huile, deux ou
trois lampes de cuivre de forme antique, un chapelet de dents de
loups et un vieux fusil. Et les petites filles allaient et venaient,
passant comme des ombres de gnômes, nous regardant de leurs
grands yeux noirs et sérieux, vaquant silencieusement aux soins du
ménage autour du feu pétillant.
Une odeur d’étable mal tenue mêlée à celle de l’huile rance et de
la fumée de bois vert emplissait et alourdissait l’atmosphère, et la
nuit était tout à fait venue.
Je ne sais depuis combien de temps je dormais, lorsque je fus
réveillé par un grand bruit confus. Près du foyer une horrible femme
accroupie frottait une casserole ; maigre et dévastée avec des
cheveux grisâtres qui s’échappaient, en mèches de crin, d’un foulard
sale enroulé sur sa tête, elle me produisit du premier coup
l’impression de ces aïeules de brigands qu’artistes et romanciers
représentent préparant au fond des cavernes le souper de la bande.
Son visage était plus criblé de trous qu’une cible et l’un de ses yeux
manquait à l’appel ; mais celui qui restait, le bon, semblait si
farouche qu’on l’eût, ma foi, crevé sans remords. Bien qu’on fût au
cœur de l’été, une demi-douzaine de gros jupons au moins
s’accrochaient à ses hanches sèches, ce qui lui faisait une énorme
croupe, contraste étrange avec la maigreur et la platitude du reste
de la charpente.
Elle grommelait je ne sais quoi entre ses dents jaunes qui
paraissaient vouloir s’échapper continuellement de cette mauvaise
bouche, apostrophant de temps à autre l’aînée des petites filles qui
n’obéissait pas assez vite aux exigences d’un affreux marmot qui, le
cul par terre, trépignait de rage, raclait la poussière de ses sales
doigts et la lançait dans la direction de sa sœur en réclamant
impérieusement du lait. Un chat famélique au poil hérissé guignait la
tasse de son œil jaune et scélérat, tandis que deux solides mâtins
de haute taille faisaient une entrée brusque et triomphante qu’un
tison ardent lancé par la vieille changea en fuite honteuse et
précipitée. Et une grande clameur emplissait la maison, jurons de
bergers, bêlements de moutons et de chèvres que dominaient les
grognements aigus de cochons.
Le troupeau rentrait.
Entraient en même temps un jeune garçon de quatorze à quinze
ans, à l’œil sournois, visiblement le fils ou le petit-fils de la sorcière,
qui s’assit dans un coin, après un brusque bonsoir ; puis, un gaillard
de mauvaise mine, chaussé d’espadrilles de peau, avec un fusil en
bandoulière, et enfin le batteur de blé. Ils s’installèrent sur le banc
faisant face au nôtre, avec des visages dépourvus d’affabilité, celui
du batteur de blé spécialement, sur lequel nos revolvers et nos
cartouchières accrochés au mur, derrière nous, paraissaient produire
une fâcheuse impression.
XII
HISTOIRE DE BRIGANDS
Enfin le souper est prêt ; souper d’anachorète. Une panade au

lait de chèvre c’est là tout le menu. Avec de tels repas les mœurs
doivent être pures. On songe aux pastorales genre Daphnis et
Chloé. Mais quelle sale Chloé que cette vieille ! Au fait, la fraîche
héroïne de Longus devint sans doute aussi une sorcière avec l’âge,
et la maugrabine qui nous sert fut peut-être une beauté jadis. Belles
dames, ce que c’est que de nous !
Je me faisais ces réflexions philosophiques en dégustant ma
panade à la gamelle commune avec la cuillère qu’on avait, pour me
la donner, arrachée de la bouche de l’affreux marmot qui réclamait
son bien avec des cris de colère. Je n’engage pas les gens
dégoûtés à s’arrêter à la venta du col de Piqueras. Il n’y passe
d’ailleurs pas deux voyageurs par an. Aussi, hôte, hôtesse et
jusqu’aux petites filles semblaient nous examiner d’un air goulu ;
nous étions une de ces proies rares que le bon Dieu envoie deci,
delà aux honnêtes hôteliers, et d’autant mieux qu’en fouillant ses
poches mon compagnon de route avait commis l’imprudence d’en
tirer deux ou trois pièces d’or.
Après la panade au lait suffisamment piquetée de belles
mouches, pain et oignon, vin à discrétion. Cependant le sommeil
nous gagne et nous nous demandons avec une certaine inquiétude
dans quel coin d’étable on va dresser nos litières ; calomnie
gratuite : on nous a préparé des lits. Par un escalier de bois auquel
manque la moitié des marches et dont le reste crève sous le pied,
l’aînée des petites filles nous guide à l’étage supérieur, munie d’une
lampe, et nous conduit à nos chambres.
Nos chambres ! C’est la première fois depuis notre entrée en
Espagne que nous avons chacun la nôtre et toutes deux éloignées
l’une de l’autre, séparées par un long corridor. Voilà qui n’est pas de
nature à nous inspirer confiance, d’autant qu’en montant l’escalier
nous avons entendu des chuchotements suspects. Nous avons nos
revolvers heureusement, décrochés bien ostensiblement, malgré
l’observation de l’amo que nous pouvions aussi bien les laisser à
leur clou.
La première chambre où s’arrête mon compagnon est une sorte
de cellule qui n’a d’ouverture que la porte. Je m’empresse de la lui
laisser, aimant les pièces où l’on peut respirer à l’aise. Je suis servi à
souhait. J’entre dans une sorte de halle ouverte à tous vents et qui
couvre une partie de l’étage inférieur.
La petite fille qui me précède avec sa lampe me prévient de faire
attention où je pose le pied. Recommandation tardive, j’avais déjà
failli disparaître deux ou trois fois dans des dessous inconnus. Le
plancher, ou du moins ce qui jadis a été le plancher, n’existe plus
qu’à l’état de carcasse et, d’entre les crevasses, montent
d’asphyxiantes buées. Des grognements et des bêlements partant
d’en bas expliquent le phénomène.
Au rebours du recoin, précédent orné d’une porte, mais privé de
fenêtres, il y a ici quatre fenêtres et pas de porte, et les fenêtres
ouvertes sur la montagne sont barrelées comme celles d’une prison.
Après des tours d’équilibriste sur des planches pourries posées
comme des ponts sur des abîmes béants, j’atteins une sorte
d’alcôve, où un lit est dressé au-dessous d’une image du grand saint
Joseph qui, la main ouverte, vous invite à y dormir sous sa bonne et
digne garde.
Comme le plancher, le lit vermoulu fait bascule. Il est, d’ailleurs,
aussi sommaire que le dîner. Deux sacs de paille ; le plus petit posé
en travers forme le traversin. Le tout recouvert d’un carré de laine et
d’un drap dont la flamme insuffisante de la lampe ne me permet pas
de vérifier la blancheur.
Je pris la lampe des mains de l’enfant, l’accrochai à la muraille à
côté d’un bénitier et me préparais non à dire mes prières, comme
vous pourriez le supposer, et comme semblait m’y engager le
vénérable époux de la Vierge Marie, mais à me débarrasser de mes
culottes, lorsque je m’aperçus que la petite fille, au lieu de se retirer
discrètement, comme il sied à une personne de son âge, restait
plantée devant moi et suivait tous mes mouvements avec ses
grands yeux noirs chargés de curiosité.
« Tu peux t’en aller, lui criai-je en mon patois, je n’ai plus besoin
de tes services. »
Mais elle ne bougea pas, paraissant s’être juré à elle-même
d’assister au coucher d’un Français.
Rapidement débarrassé de mon veston, de mon gilet, de mes
chaussures, de ma ceinture de laine, j’avais placé mon revolver sous
mon traversin.
Il ne me restait donc plus que le vêtement que les Anglaises
appellent l’inexpressible, mais que, n’étant pas Anglaise, la niña
n’avait nulle raison pour ne pas exprimer, et qu’elle exprima
d’ailleurs fort bien, voyant mon hésitation, en me demandant avec
une sorte d’impatience si je couchais avec mes calzones.
Assez surpris de la question, je lui fis entendre que je n’avais pas
l’habitude de retirer mes culottes devant d’aussi jeunes demoiselles,
sur quoi elle s’avança vers mon lit et se saisit de la lampe.
Je crus un instant qu’elle allait l’éteindre afin de ménager ma
pudeur, mais elle n’avait d’autre but que de l’emporter, ce qu’elle fit
rapidement en me souhaitant une bonne nuit.
« Hé ! lui criai-je, où vas-tu ?
— Me coucher, répliqua-t-elle.
— Pourquoi emportes-tu ma lampe ?
— Parce que maman me l’a dit.
— Elle est bien aimable, ta maman, mais j’en ai besoin.
— Pour quoi faire ? demanda-t-elle.
— Tu es bien curieuse. Mais puisque tu es si curieuse, je vais
l’être autant que toi. Indique-moi certain endroit indispensable,
surtout après les repas de panade au lait.
— Là ! dit-elle.
— Où çà, là ?
— Eh bien là ! ici ! là ! où vous voudrez. »
Et elle me montra les crevasses du plancher.
Il était bien inutile de lui disputer la lampe. Je m’aperçus bientôt
qu’elle n’avait que pour quelques minutes de vie, et, en effet, une
dizaine à peine écoulée il ne resta qu’une mèche charbonneuse.
Une heure environ se passa.
Sur ce squelette de plancher, il était dangereux de s’aventurer
sans lumière. J’avais bien un bout de bougie dans mon sac, mais
ma boîte d’allumettes était restée entre les mains de notre hôte qui
me l’avait demandée pour allumer une cigarette.
Je me décidai d’aller en emprunter à mon compagnon.
M’assurant du terrain avec le pied avant de l’y poser, comme font les
bons chevaux dans les mauvais chemins, je me guidai sans trop
d’encombre jusqu’à son réduit.
Il ronflait déjà comme un juste, et tandis que je tâtonnais,
cherchant ses allumettes, en évitant de troubler son somme,
j’aperçus, par une large crevasse, un filet de lumière, en bas, et
l’ombre projetée sur le mur d’un homme qui chargeait
silencieusement son fusil. Puis l’ombre se doubla ; se tripla ; se
quadrupla ; le rayon lumineux se déplaça, les marches de l’escalier
craquèrent, et je distinguai l’horrible vieille, une lanterne à la main,
précédant une troupe de brigands armés.
Les deux hommes, le fils, la mère. La bande au complet.
Je me remémorais en vain, pour me rassurer, l’aventure des faux
brigands que raconte si plaisamment Courier, lorsqu’il voyageait en
Calabre. La mienne s’offrait toute semblable. Rien n’y manquait : la
nuit, l’endroit isolé, le désert environnant, l’aspect farouche de nos
hôtes, leurs armes, la vieille scélérate, jusqu’aux deux énormes
chiens qui, sans doute attachés en bas, près de la porte, coupaient
toute retraite ; jusqu’à mon compagnon qui, rompu de fatigue,
dormait comme un sourd.
Ils n’étaient pas une quinzaine, il est vrai, comme les
charbonniers de Paul-Louis, et je n’avais pas entendu le mari dire à
sa femme : « Faut-il les tuer tous deux ? » mais je voyais
distinctement celui-ci lever et baisser le bras pour ordonner de
marcher doucement, geste qu’il appuyait du mot « chuto ! chuto ! »
prononcé à voix basse par deux fois.
Que diable venaient faire ces gens ? Évidemment ils ne venaient
pas avec l’intention de nous inviter à une noce. Je pensais bien au
jambon de l’histoire de l’illustre pamphlétaire tourangeau, mais il n’y
avait pas de jambon appendu dans ces soupentes et d’ailleurs ce
n’est nulle part la coutume de les décrocher à coups de fusil.
Il va sans dire que réflexions et réminiscences eurent la durée
d’un éclair, car les brigands montaient toujours, avec le moins de
bruit possible ; mais leurs pieds quoique chaussés d’espadrilles font
craquer quand même les marches pourries.
Je songe que mon revolver est resté là-bas, sous mon traversin.
Il faut y arriver sans encombre. Je secoue brusquement mon
compagnon, qui répond par un gémissement et fait un demi-tour sur
l’autre oreille. Au risque de me rompre le cou ou les jambes, ou de
passer au travers du plancher, trébuchant, basculant et me heurtant,
j’atteins ma couche.
La bande est sur mes talons : elle a dû entendre le bruit de ma
course et n’ayant pas à s’inquiéter de mon compagnon qui ronfle,
arrive à ma chambre presque en même temps que moi.
A la faible lueur de la lanterne, que porte la vieille gueuse, je vois
les faces patibulaires. Je ne me suis pas trompé. Ils sont bien tous
trois armés de fusils. Notre hôte, en éclaireur, se dirige vers l’alcôve.
« Chuto ! chuto ! dit la sorcière ; ne le réveillez pas.
— Pugnatera ! réplique le second brigand, il va bien se réveiller
tout à l’heure ! »
Et tous d’ouvrir la bouche en un rire silencieux et diabolique.
« Mon affaire est faite ! pensais-je. Aussi quelle diable d’idée de
passer dans ces gorges et de nous arrêter dans cet antre. Et cet
animal qui ronfle là-bas !
— Gare au revolver ! murmura la vieille. La niña à vu l’homme le
placer sous son traversin. Attention !
— Ah ! la petite gueuse, me dis-je, c’est donc cela qu’elle
guettait ! » J’ai la main posée dessus, le doigt sur la détente et au
même moment avec quelque étonnement on me voit debout, appuyé
contre mon lit.
« Que quiere usted ? m’écriai-je d’une voix terrible.
— Chuto ! chuto ! réplique le premier brigand avec un grand
geste. Pas de bruit. »
Je répète ma question.
« Rien, dit l’homme, nous ne voulons rien à vous. Je voulais
seulement voir si vous dormiez. »
Ils se répandent dans la vaste pièce, occupant trois des fenêtres
chacun avec son fusil, comme gens assiégés s’apprêtant à
repousser une attaque.
« Qu’est-ce qu’il y a donc ? demandai-je à la vieille qui entrait
dans l’alcôve avec sa lanterne pour la placer flamme au mur de
façon que la lumière ne pût être aperçue du dehors.
— Ah ! les brigands, répondit-elle, j’espère qu’on va en tuer deux
ou trois.
— Qui donc ? On attaque la venta ? »
Elle me prit la main, me guida jusqu’à la fenêtre restée vide.
« Vous allez les voir. Ils sont là, tenez, tenez… comptez… un,
deux, trois, quatre. Je ne parle pas des capons embusqués, là-bas,
dans les broussailles et qui attendent le signal des camarades pour
se mettre en train. Ole ! ole ! »
Dans la belle nuit claire, je vis se glisser quatre formes allongées
semblables à des silhouettes de gros épagneuls. Et presque au
même instant, trois détonations retentirent, suivies de terribles
hurlements auxquels répondirent les aboiements furieux des chiens
enfermés dans l’étable.
« Bien ! s’exclama la vieille. Deux ! »
Deux loups en effet se débattaient, pattes en l’air, dans la
poussière du chemin, tandis que mon compagnon, réveillé en
sursaut par l’effroyable bruit, accourait en chemise, œil effaré et
revolver au poing.
« Vaya ! vaya ! aségûrese ! dit en riant notre hôte. Là ! là !
tranquillisez-vous ! »
Puis se tournant vers moi : « Ça les dégoûtera pour quelques
jours. »
Le lendemain, remis des émotions de la nuit, nous partons en
même temps que les troupeaux, après un déjeuner de panetela
restant du souper.
Nos hôtes qui, à la lumière fumeuse, nous ont paru avoir des
mines de fieffés coquins semblent au contraire de fort honnêtes
gens. Si la matrone, avec son œil crevé, n’est pas un échantillon
séduisant du beau sexe des Castilles, elle a l’air moins revêche et
moins sordide que la veille, et la vue de quelques pesetas glissées
dans sa main adoucit la dureté de son unique prunelle.
Quant au maître de céans, il nous raconte que les loups lui ont
encore dévoré un mouton le soir précédent, au moment où le
troupeau rentrait, et étranglé deux chiens depuis le commencement
de l’été.
Son acolyte, l’homme au fusil, qui n’est autre qu’un honnête
cantonnier du voisinage, est venu à la rescousse dans sa haine des
loups. Chaque année, il est obligé de quitter sa maison dès que
tombent les neiges pour se réfugier à Pajarès, et elles commencent
dès septembre pour ne cesser qu’en avril ou mai ; et chaque année
il trouve sa porte enfoncée et sa maison envahie. Les loups entrent
parfois, par bandes, dans le village de Pajarès, et poussent l’audace,
comme on l’a vu, jusqu’à rôder près des étables, même dans les
nuits d’été. « Que voulez-vous, dit philosophiquement notre hôte : Lo
que ha de ser no puede faltar », variante du vieux proverbe fataliste
arabe : « Ce qui est écrit est écrit. »
Et ainsi se termine mon histoire de brigands.

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List of boxes viii

The investigative approach 1

Fundamental laboratory techniques 61

Laboratory techniques 121

Classical techniques 177

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Instrumental techniques 215

Information technology and library resources 373

Analysis and presentation of data 435

Study and examination skills 521

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Communicating information 573

Answers to study exercises 609

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2.1 How to perform a risk matrix analysis 8

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30.5 Analysis of a sample: dilution factor 230

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5 1.1 Example of using the algebraic rules of Table 51.2 465

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43 Using online resources

Information and communication technology (ICT) is vital in the modern aca-

Definitions of key terms and

ful hints and practical advice,

and are highlighted in the text Understanding the technology – you

features of methodology. wireless network can be complex, but

the hardware. White and Downs (2014) online communication

Information technology and library resources 389

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