Chapter 1
Chapter 1
Chapter 1
K Chapter 1 Exercise k
A B C D E
42.5 39.8 43.5 35.0 42.2
41.6 43.6 42.8 43.0 41.6
42.1 42.1 43.8 37.1 42.0
41.9 40.1 43.1 40.5 41.8
41.1 43.9 42.7 36.8 42.6
42.2 41.9 43.3 42.2 39.0
2. Using the same sample and method as in question 1, laboratory A makes six further determinations of the
albumin concentration, this time on six successive days. The values obtained are 41.5, 40.8, 43.3, 41.9,
42.2 and 41.7 g l−1 . Comment on these results.
6. The following data give the recovery of bromide from spiked samples of vegetable matter, measured by
using a gas-liquid chromatographic method. The same amount of bromide was added to each specimen.[4]
(a) Test whether the recoveries from the two vegetables have variances which differ significantly.
(b) Test whether the mean recovery rates differ significantly.
7. The following results show the percentage of the total available interstitial water recovered by centrifuging
samples taken at different depths in sandstone.
Show that the percentage of water recovered differs significantly at different depths.
8. The following table gives the results of the determination of chromium in organic materials for two
different methods.
Method 1 mean = 2.15 s.d. = 0.26
Pine needles:
Method 2 mean = 2.45 s.d. = 0.14
Method 1 mean = 5.12 s.d. = 0.80
Beech leaves:
Method 2 mean = 7.27 s.d. = 0.44
Method 1 mean = 23.08 s.d. = 2.63
Aquatic plant:
Method 2 mean = 32.01 s.d. = 4.66
In each case the mean is the average of five values. For each material test whether the mean results
obtained by the two methods differ significantly
2
1.4 Calibration Methods in instrumental analysis
9. Six analysts each made six determinations of the paracetamol content of the same batch of tablets [5].
The results are shown below:
(a) Test whether there is any significant difference between the means obtained by the six analysts.
10. A new flame atomic-absorption spectroscopic method of determining antimony in the atmosphere was
compared with the recommended calorimetric method [6]. For samples from an urban atmosphere the
following results were obtained:
Concentration, ng ml−1 0 5 10 15 20 25 30
Absorbance 0.003 0.127 0.251 0.390 0.498 0.625 0.763
a Determine the slope and intercept of the calibration plot, and their confidence limits
b Estimate the confidence limits for the silver concentrations in
i a sample giving an absorbance of 0.456 in a single determination, and
ii a sample giving absorbance values of 0.308, 0.314, 0.347 and 0.312 in four separate analyses.
c Estimate the limit of detection of the silver analysis.
3
1.4 Calibration Methods in instrumental analysis
12. The gold content of a concentrated seawater sample was determined by using atomic-absorption spec-
trometry with the method of standard additions. The results obtained were as follows.
Gold added,
ng per ml of
concentrated
sample 0 10 20 30 40 50 60 70
Absorbance 0.257 0.314 0.364 0.413 0.468 0.528 0.574 0.635
Estimate the concentration of the gold in the concentrated seawater, and determine confidence limits for
this concentration.
13. In a study of the complex formed between europium (III) ions and pyridine-2, 6-dicarboxylic acid (DPA),
the absorbance values of solutions containing different DPA:Eu concentrations were determined, with the
following results: [7]
Use these two rows of data to determine the slopes and intercepts of two separate straight lines. Estimate
their intersection point and its standard deviation, thus determining the composition of the DPA-europium
complex formed.
4
Bibliography
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[3] Qiu Xing-Chu and Zhu Ying-Quan. “Spectrophotometric study of the reaction of titanium (IV) with
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[4] John A Roughan, Patricia A Roughan, and John PG Wilkins. “Modified gas-liquid chromatographic method
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[5] Andrew D Trafford et al. “A rapid quantitative assay of intact paracetamol tablets by reflectance near-
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A806629I.
[6] JR Castillo et al. “Flame atomic-absorption spectroscopic determination of antimony in atmospheric
particulates by using direct atomisation of the covalent hydride”. In: Analyst 107.1281 (1982), pp. 1488–
1492. url: https://doi.org/10.1039/AN9820701488.
[7] Nadine Arnaud, Eric Vaquer, and Joseph Georges. “Comparative study of the luminescent properties
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[8] J.N. Miller and J.C. Miller. Statistics and Chemometrics for Analytical Chemistry. Pearson/Prentice Hall,
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