External calibration

1. The determination (by triplicate) of lithium, calcium, lead and copper in a serum sample was performed
by atomic absorption spectroscopy. Determine the concentration (in ppm) of lithium, calcium, lead and
copper in the analyzed serum sample

Concentration of Analytical
Element Technique Sample Preparation
Standards in mmol/L Signal
0.25 100
0.20 81
0.15 61
Flame Atomic 1 mL serum is diluted
0.10 41
Absorption with 9 mL deionized
Li 0.05 20
Spectroscopy water
0.00 0
( = 678 nm) (total: 10 mL)
Serum sample 1 38
Serum sample 2 41
Serum sample 3 37

Concentration of Analytical
Element Technique Sample Preparation
Standards in mmol/L Signal
0.0 0
9.5 mL of 4%. 1.5 43
triclhoroacetic acid are 2.0 58
Flame Atomic
added to 0.5 mL 2.5 72
Absorption
Ca serum. (total: 10 mL) 3.0 85
Spectroscopy
Centrifugation and 3.5 100
( = 422.7 nm)
aspiration of Serum sample 1 69
supernatant solution Serum sample 2 72
Serum sample 3 73

Concentration of Analytical
Element Technique Sample Preparation
Standards in mg/mL Signal
Blank 0.00
0.25 5.4
Graphite Furnace 0.50 10.9
Flame Atomic Direct introduction in 1.00 25.2
Pb
Absorption the oven 2.00 48.2
( = 238.2 nm) Serum sample 1 23.7
Serum sample 2 22.0
Serum sample 3 24.5

Concentration of Analytical
Element Technique Sample Preparation
Standards in mg/mL Signal
Blank 0.0
Digestion of 2 mL of 0.5 13
Graphite Furnace sample in 5 mL of an acid 1.0 25.1
Flame Atomic mixture HNO3/H2SO4. 1.5 45.9
Cu
Absorption (total 5 mL) 2.5 64.3
( = 324.8 nm) Then, 1:10 dilution with Serum sample 1 18.5
deionized water. Serum sample 2 17.0
Serum sample 3 19.0
 Internal Standard

2.- Calcium can be analyzed using lithium as internal standard. The following emission intensities
were obtained for calcium in a soil sample. Sample treatment included solving 1 g of soil in a 100
mL flask. What is the concentration of calcium in ppm in the soil sample?

[Ca], ppm 1 2 3 4 5 6 Soil sample

Intensity Ca 29 41.4 50.8 60.7 76.4 83.5 74
Intensity Li 87 88 84 81 89 85 88.5

MORE EXAM TYPE 3.- The use of the voltammetric anodic dissolution technique is appropriate for the determination
of cadmium in water using Cu2+ as internal standard. Five 100 mL volumetric flasks, each
containing 1 mL of a 1.0x10-4 M solution of CuSO4, and varying amounts (specified in the table
below) of a standard solution 1.00x10-4 M of cadmium were prepared.

The sample was prepared by pipetting 50 mL of the water sample and adding 1 mL of a 1.0x10-4
M solution of CuSO4. Each solution was brought to a 100 mL volumetric mark with deionized
water and measured. The signals specified in the table were observed:

Calculate the cadmium concentration in the sample.

Copper Peak Cadmium Peak

Volume stock solution Cd (mL)
(mA) (mA)
0 14.8 17.5
1 15.5 22.4
2 17.0 34.4
5 16.4 61.7
10 16.8 112.0

Water sample 16.2 57.7

Standard Addition

4.- An analyst determines the concentration of potassium in a sample using the standard addition
method. The readings obtained are shown in the table. The sample was prepared by dissolving
1 g of the sample in a 100 mL volumetric flask. In order to prepare the calibration by the standard
addition method, 10 mL of this sample solution were added to 100 mL volumetric flasks. Before
taking to the line, increasing volumes of a standard stock solution were added to each flask.
Determine the concentration of potassium in the sample in ppm and percentage.

[K], ppm 0 1 2 5 10 20 50
Intensity 18.0 19.5 21.0 25.5 33.0 48.0 93.0

5.- The determination of iron in wines by atomic absorption spectrophotometry was carried out
using the standard addition method. 10 ml of wine were placed in five 50 ml volumetric flasks.
Subsequently, 0, 5, 10, 15 and 20 ml of an iron standard solution containing 10 ppm of Fe were
added to each of them. They were then made up with deionized water and the atomic absorbance
of the iron was measured. The values of 0.040, 0.062, 0.081, 0.102 and 0.135 respectively were
obtained. Obtain the equation of the regression line and calculate the concentration of iron in the
wine (in mg / L).

6.- The measurement of Li in brine (saline water) is used by geochemists as a means to determine
the origin of this fluid in the oil fields. The flame atomic emission of Li is subjected to interference
due to the dispersion, ionization and emission of other elements in the matrix. For this reason Li
was determined in a marine sediment using the standard addition method. With the data in the
table, calculate the concentration of Li in the sample. The concentration of the stock standard
solution was 1.62 μg / mL.

Sample Volume of Final Emission Intensity

(mL) standard (mL) Volume (mL) (arbitrary units)
10 0 100 309
10 5 100 452
10 10 100 600
10 15 100 765
10 20 100 906
%
SIGNAL

concentrate
( ppm )
ppm
 It is
dividing
Lou
by

Mean
standard devo

significant
figure
61800 ± 700
Atomic
weight
calcium
SO MULTIPLY BY 1000
 TAKE THIS ONE AWAY

SO THIS IS NOT CORRECT

Concentration of Li in
the sea water sample
= 1.2%