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Gravimetric Analysis Tutorial

Key Concepts

  Gravimetric analysis is the quantitative isolation of a substance by precipitation and

weighing of the precipitate.1
  An analyte is the substance to be analysed.
  A precipitating reagent is the reactant used to precipitate the analyte.2
  The precipitate must be a pure substance of definite chemical composition.
  One advantage of gravimetric analysis compared to volumetric analysis (titrimetric
analysis) is that there is greater likelihood of any impurities being seen, and therefore
a correction can be applied.
  One disadvantage of gravimetric analysis is that it is generally more time-consuming.
  Gravimetric analysis can be used to determine the:

(i) percentage of sulfate in lawn fertiliser

(ii) concentration of chloride in water

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General Procedure:

1. Weigh the sample to be analysed

2. Dissolve the sample in a suitable solvent, eg, water
3. Add an excess of the precipitating reagent to precipitate the analyte
4. Filter the mixture to separate the precipitate from the solution3
5. Wash the precipitate to remove any impurities4
6. Dry the precipitate by heating to remove water
7. Cool the precipitate in a dessicator to prevent the precipitate absorbing moisture from the air
8. Weigh the cooled precipitate
9. Repeat the drying and weighing process until a constant mass for the precipitate is achieved
10. Calculate the percent by mass of analyte in the sample
General calculation of the percent by mass of analyte in a sample:

1. Write the balanced chemical equation for the precipitation reaction

2. Calculate the moles of precipitate: moles = mass ÷ molar mass
3. Calculate moles of analyte from the balanced chemical equation using the mole ratio of analyte
: precipitate
(also known as the stoichiometric ratio of analyte to precipitate)
4. Calculate mass of analyte: mass = moles × molar mass
5. Calculate percent by mass of analyte in sample: (mass analyte ÷ mass sample) × 100

Sources of Error:

 Incomplete precipitation results in a value for the percentage of analyte in the sample
that is too low.
 Incomplete drying of the sample results in a value for the percentage of analyte in the
sample that is too high
 Other ions in the sample may also be precipitated resulting in a value for the
percentage of analyte in the sample that is too high

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Worked Example
Question:

A 2.00 g sample of limestone was dissolved in hydrochloric acid and all the calcium present in the
sample was converted to Ca2+(aq).

Excess ammonium oxalate solution, (NH4)2C2O4(aq), was added to the solution to precipitate the
calcium ions as calcium oxalate, CaC2O4(s).

The precipitate was filtered, dried and weighed to a constant mass of 2.43 g.

Determine the percentage by mass of calcium in the limestone sample.

Answer:

1. Wite the balanced chemical equation for the precipitation reaction:

Ca2+(aq) + C2O42-(aq) → CaC2O4(s)

2. Calculate the moles of calcium oxalate precipitated.

 moles(CaC2O4(s)) = mass ÷ molar mass

moles(CaC2O4(s)) = 2.43 ÷ (40.08 + 2 x 12.01 + 4 x 16.00)

moles(CaC2O4(s)) = 2.43 ÷ 128.10

moles(CaC2O4(s)) = 0.019 mol

3. Find the moles of Ca2+(aq).

From the balanced chemical equation, the mole ratio of Ca2+ : CaC2O4(s) is 1 : 1

So, moles(Ca2+(aq)) = moles(CaC2O4(s)) = 0.019 mol

4. Calculate the mass of calcium in grams

mass (Ca) = moles × molar mass

mass (Ca) = 0.019 × 40.08 = 0.76 g

5. Calculate the percentage by mass of calcium in the original sample:

%Ca = (mass Ca ÷ mass sample) × 100

%Ca = (0.76 ÷ 2.00) x 100 = 38%

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Problem Solving using StoPGoPS method

Question:

A particular water soluble fertiliser contains phosphorus in the form of phosphate ions,
PO43-.
A student used the following procedure to determine the percentage of phosphorus in a
sample of soluble fertiliser.

1. 5.17 g of fertiliser was added to a 250.0 mL volumetric flask and water was added to
make it up to the mark.
2. 20.00 mL of this solution was pipetted into a conical flask.
3. A slight excess of precipitating agent was added to precipitate the phosphate ions as
MgNH4PO4.
4. The precipitate was filtered, washed with water and then converted by heating into
Mg2P2O7
 5. The mass of Mg2P2O7 was 0.0312 g

Calculate the percentage by mass of phosphate in the fertiliser.

STOP STOP! State the Question.

What is the question asking you to do?

  Calculate the percentage by mass of phosphate in the fertiliser.

%(PO43-) = ? %

PAUSE PAUSE to Prepare a Game Plan

(1) What information (data) have you been given in the question?

mass of fertiliser = m(fertiliser) = 5.17 g

initial volume of solution = Vi = 250.0 mL

volume of solution used in experiment = Vf = 20.00 mL

mass of Mg2P2O7 = m(Mg2P2O7) = 0.0312 g

(2) What is the relationship between what you know and what you need to
find out?
 
(i) moles(Mg2P2O7) = mass(Mg2P2O7) ÷ molar mass(Mg2P2O7)

(ii) 2P (from PO43-) → Mg2P2O7

(iii) In 20.00 mL sample solution: moles(P) = 2 × moles(Mg2P2O7)

(iv) moles(P) in 250.0 mL solution = moles(P) in 20.00 mL sample × 250.0/20.00

(v) each mole PO43- contains 1 mole of P

(vi) mass(PO43-) = moles(PO43-) × molar mass(PO43-)

(vii) %(PO43-) = 100 × mass(PO43-)/mass(fertiliser)

GO GO with the Game Plan

  (i) moles(Mg2P2O7) = mass(Mg2P2O7) ÷ molar mass(Mg2P2O7)

mass(Mg2P2O7) = 0.0312 g (given)

molar mass(Mg2P2O7) = (2 × 24.31) + (2 × 30.97) + (7 × 16.00) = 222.56 g mol-1
 moles(Mg2P2O7) = 0.0312 ÷ 222.56 = 1.40 × 10-4 mol

(ii) 2P (from PO43-) → Mg2P2O7

mole ratio P : Mg2P2O7 is 2:1

(iii) In 20.00 mL sample solution: moles(P) = 2 × moles(Mg2P2O7)

moles(P) = 2 × 1.40 × 10-4 = 2.80 × 10-4 mol

(iv) moles(P) in 250.0 mL solution = moles(P) in 20.00 mL sample × 250.0/20.00

moles(P) = 2.80 × 10-4 × 250.0/20.00 = 3.50 × 10-3 mol

(v) each mole PO43- contains 1 mole of P

moles(PO43-) = moles(P) = 3.50 × 10-3 mol

(vi) mass(PO43-) = moles(PO43-) × molar mass(PO43-)

moles(PO43-) = 3.50 × 10-3 mol

molar mass(PO43-) = 30.97 + 4 × 16.00 = 94.97 g mol-1

mass(PO43-) = 3.50 × 10-3 × 94.97 = 0.332 g

(vii) %(PO43-) = 100 × mass(PO43-)/mass(fertiliser)

%(PO43-) = (0.332/5.17) × 100 = 6.42 %

PAUSE PAUSE to Ponder Plausibility

Is your answer plausible?

Approximate by rounding off the numbers to the nearest 10 (or 5):

n(Mg2P2O7) ≈ (5 × 10-2 g) ÷ (2 × 102) g mol-1 ≈ 2.5 × 10-4 mol
  n(P) ≈ 2 × 2.5 × 10-4 mol = 5 × 10-4 mol
n(PO43-) ≈ 5 × 10-4 mol
m(PO43-) ≈ 5 × 10-4 mol × (30 + 60 g mol-1) ≈ 5 × 10-4 × 100 ≈ 5 × 10-2 g
%(PO43-) ≈ (0.05/5) × 100 ≈ 1%
Our answer of 6.42% is in the same region as the approximated 1% so we are
reasonably confident out answer is correct.

STOP STOP! State the Solution

  Percentage by mass of phosphate ion in fertiliser is 6.42 %

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1. The separation of the element or the compound containing it may done a number of different ways, precipitation
is one of the most common. Other methods include volatilisation and electro-analytical methods.

2. The precipitate formed must be stable and must be so  slightly soluble that no appreciable loss occurs when
the precipitate is separated by filtration and weighed.

3. The particles making up the precipitate must be large enough so that they do not pass through the filtering
medium, and, the must remain larger than the pore size of the filter medium during the washing process.
Ordinary quantitative filter paper will retain particles up to a diameter of about 10 μm.

4. Washing removes impurities from the surface of the precipitate particles but will not remove occluded foreign
substances.

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Page Reference

AUS-e-TUTE, 8 April 2018,

Gravimetric Analysis Chemistry Tutorial,
viewed 17 November 2020,
https://www.ausetute.com.au/gravimetric.html

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Follow
Example: Calculate the amount of sulphate as barium sulphate from sodium sulphate.
Solution of sodium sulphate (Na2SO4) is treated with solution of barium chloride (BaCl2) to get
precipitates of barium sulphate (BaSO4). The precipitates are then washed, dried and ignited to get free
from impurities and then weighed.
 
Na2SO4 + BaCl2 → BaSO4 + 2 NaCl
 
Mol. Weight of BaSO4 = 233.42 gm
Mol. Weight of SO4- = 96.06 gm
 
Suppose obtained weight of BaSO4 precipitates = X · gm
233.42 gm of BaSO4 = 96.06 gm of SO4- ions
X · gm of BaSO4 = ?
BaSO4 = 96.06 · X / 233.32 = 0.411X gm of SO4- ions
 
Suppose 25 ml solution is consumed, then
 
25 ml solution contains = 0.411X gm of SO4- ions
1000ml solution conatins?
1000ml solution conatins = 0.411X · 1000 / 25  = 16.44X gm of SO4- ions
 
Example: Calculate the amount of zinc oxide from zinc sulphate.
A solution of zinc sulphate is boiled to convert it into zinc carbonate by adding solution of sodium
carbonate. Sodium carbonate is added to precipitate zinc completely as zinc carbonate. Precipitates of
zinc carbonate is boiled for few minutes to convert it into zinc oxide and collected in a tarred Gooch
crucible. Precipitates are washed with hot water until it gets free from alkali and then dried, ignited and
weighed to a constant weight.
 
ZnSO4 + Na2CO3 → ZnCO3 + Na2SO4
 
ZnCO3 → ZnO + CO2
 
ZnSO4 = ZnCO3 = ZnO
ZnSO4 = ZnO
 
Mol. Weight of ZnSO4 = 168 gm
Mol. Weight of ZnO = 81.38 gm
 
81.38 gm of ZnO = 168 gm of ZnSO4
1 gm of ZnO =?
= 168 · 1 / 81.38
= 1.984 gm
 
Example: Calculate the amount of Boric acid from Borax.
Borax is an alkaline substance, and reacts with conc. HCl to form Boric acid. Boric acid is freely soluble in
boiling water and precipitated out in cold water. To get high grade of Boric acid, Borax is treated with
conc. HCl as it is volatile in nature and won’t left any residual traces on crystal surface of Boric acid.
 
Weight and dissolve 5 gm of Borax in 15 ml of distilled water. Add 7 ml of conc. HCl, mix thoroughly with
glass rod and mark the original volume with glass rod. Evaporate the solution till the volume reduces to
half of the original volume. Allow to cool at room temperature. Keep it aside for few min and add ice
water. Filter the residue under suction and dry it in air. Weight the compound preparation.
 
Na2B4O7.10H20 → 4H3BO3 + 5H20 + 2NaCl
 
Mol wt of Borax = 381.37gm
Mol wt of Boric acid = 61.83gm
Practical yield: X gm
 
381.37 gm of Borax = 4 × 61.83 gm of Boric acid
X gm of Borax = ?
= X · 4 · 61.83 / 381.37
= 0.674X gm of Boric acid

 Exercises in Titrimetric Analysis

1. A 750 mg sample of iron ore was dissolved in acid and treated to oxidize all of the iron to ferric iron. After dissolving any remaining
oxidizing agent, excess KI was added and the liberated I was titrated with 0.07500M Na S O . If the ore sample contains 15.67 % Fe,
2 2 2 3

how many ml of the titrant would be needed?

2Fe       +       2I                 2Fe       +       I
3+ - 2+
2

I         +      2S O                                 2I           +       S O
2 2 3
2- -
4 6
2-

2. A 300.0 mg sample containing H PO and inert was diluted with water and titrated with 0.0500M NaOH. The end point was reached
3 4

after 29.00 ml of titrant was added. Calculate the percent H PO in the sample.                   H PO       +      NaOH            products
3 4 3 4   

3. A sample of an antihistamine, brompheniramine maleate, weighing 4.6330 g was dissolved in alcohol and decomposed with metallic
sodium.  The resulting solution was treated with 10.00 ml of 0.2500 M AgNO , an amount sufficient to precipitate all of the liberated
3

bromide ion as AgBr.  The excess AgNO   was titrated with 0.1214 MKSCN, requiring 14.42 mL to reach the end point:         
3

4. Ag     +  SCN   --------------------  AgSCN(s)

+ -

    Calculate the % Br in the sample.  What additional piece of information is needed to determine the percentage of the antihistamine in
the sample?

5. A sample of an antihistamine, brompheniramine maleate, weighing 4.6330 g was dissolved in alcohol and decomposed with
metallic sodium.  The resulting solution was treated with 10.00 ml of 0.2500 M AgNO , an amount sufficient to precipitate3
 all of the liberated bromide ion as AgBr.  The excess AgNO   was titrated with 0.1214 MKSCN, requiring 14.42 mL to reach 3

the end point:

Ag     +  SCN   --------------------  AgSCN(s)

+ -

Calculate the % Br in the sample.  What additional piece of information is needed to determine the percentage of the
antihistamine in the sample?

6. During the titration of an HClO solution with 0.1032 M NaOH, quantitative analysis student Alcohol became distracted and
4

overshoots the end point.  A fellow student, I.M. Smart, suggested that he simply record the present volume of NaOH
added the titrate the excess with a standard acid solution.  If the original sample volume was 25.00 mL,  the volume of
NaOH added was 28.06 mL, and it took 3.47 mL of 0.1094 M HCl to back titrate the NaOH, calculate the molar
concentration of the original HClO solution. 4

7. A sodium thiosulfate solution  can be standardized by using it to titrate the iodine liberated by the action of excess Kl on a
known mass of primary standard K Cr O : 2 2 7

Cr O   +  61   +  14H   ------- 2Cr   + 31   + 7H O

2 7
2- - + 3+
2 2

                I   +  2S O   -------------------------- 21   + S O

2 2 3
2- -
4 6
2-

 
   

Calculate the molar concentration of the sodium thiosulfate solurion if 31.47 mL of this solution were required to titrate a
sample prepared using 0.2177 g of pure K Cr O 2 2 7:

8. The owner of a swimming pool  is offered what appears to be an exceptionally good deal on some concentrated
muriatic acid (HCl).  The solution is supposed to be 31.25% HCl by weight.  The store owner has some suspicion about
the seller and decides to have a sample analyzed before agreeing to make a purchase.  The chemist he hired determined
the density of the solution to be 1.367 g/ml.  Then a 5.00 ml aliquot of the acid was diluted to 250 ml.  A 50.0 ml
aliquot of the diluted sample required 22.5 ml of 0.300 M NaOH for titration to the phenolphthalein end point.  What is
The percent HCl in the 5.0 ml aliquot solution is

9. A 0.1428-gram sample containing CaCO was pulverized and heated in a closed system causing the  3

    evolution  of CO 2

                CaCO ----------------------------CaO    + CO

3 2

A stream of nitrogen was used to sweep the CO2 into 100.0 ml of 0.05172 M NaOH solution:

                CO   + 2NaOH    ----------------     Na CO   + H O

2  2 3 2

                HCl    +  NaOH    ---------------     NaCl   +   H O 2

The excess NaOH is titrated and required 28.14 ml of 0.1788 M HCl.  What is The percent of CaCO in the sample is 3

10. A 1.00 g sample containing  KHC O ,  H C O and impurities required 46.48 ml of 0.0980 M NaOH for titration.  A
2 4 2 2 4

duplicate sample required 48.35 ml of 0.0220 M  KMnO for titration in acid solution. Calculate the % of  KHC O ,  and 4 2 4

H C O in the sample
2 2 4

5C O   -  2MnO -   +  16H ---------------------- 2Mn     + 10CO + 8H O

2 4
-2
4
+ +2
2 2

        2NaOH    +  H C O   --------------- Na C O     +   2H O

2 2 4 2 2 4 2
 11. The concentration of CO  in air is determined by an indirect acid–base titration. A sample of air is bubbled through a
2

solution containing an excess of Ba(OH) , precipitating BaCO . The excess Ba(OH)  is back titrated with HCl. In a
2 3 2

typical analysis a 3.5-L sample of air was bubbled through 50.00 mL of 0.0200 M Ba(OH) . Back titrating with 0.0316 2

M HCl required 38.58 mL to reach the end point. Determine the ppm CO  in the sample of air given that the density of
2

CO  at the temperature of the sample is 1.98 g/L.

2

Ba(OH)2 + CO2 = BaCO3 + H2O

12. The protein in a 1.2846-g sample of an oat cereal is determined by a Kjeldahl analysis. The sample is digested with
H SO , the resulting solution made basic with NaOH, and the NH  distilled into 50.00 mL of 0.09552 M HCl. The
2 4 3

excess HCl is back titrated using 37.84 mL of 0.05992 M NaOH. Given that the proteins in grains average 17.54% w/w
N, report the %w/w protein in the sample.

13. The purity of a synthetic preparation of methylethyl ketone, C H O, is determined by reacting it with hydroxylamine
3 8

hydrochloride, liberating HCl. In a typical analysis a 3.00-mL sample was diluted to 50.00 mL and treated with an
excess of hydroxylamine hydrochloride. The liberated HCl was titrated with 0.9989 M NaOH, requiring 32.68 mL to
reach the end point. Report the percent purity of the sample given that the density of methylethyl ketone is 0.805 g/mL.

14. The amount of calcium in physiological fluids can be determined by a complexometric titration with EDTA. In one
such analysis a 0.100-mL sample of a blood serum was made basic by adding 2 drops of NaOH and titrated with
0.00119 M EDTA, requiring 0.268 mL to reach the end point. Report the concentration of calcium in the sample as
milligrams Ca per 100 mL.

Ca  + EDTA  → CaEDTA
2+ 4- 2-

15. After removing the membranes from an eggshell, the shell is dried and its mass recorded as 5.613 g. The eggshell is
transferred to a 250-mL beaker and dissolved in 25 mL of 6 M HCl. After filtering, the solution containing the
dissolved eggshell is diluted to 250 mL in a volumetric flask. A 10.00-mL aliquot is placed in a 125-mL Erlenmeyer
flask and buffered to a pH of 10. Titrating with 0.04988 M EDTA requires 44.11 mL to reach the end point. Determine
the amount of calcium in the eggshell as %w/w CaCO . 3

16. The concentration of cyanide, CN , in a copper electroplating bath can be determined by a complexometric titration
–

with Ag , forming the soluble Ag(CN)  complex. In a typical analysis a 5.00-mL sample from an electroplating bath is
+
2
–

transferred to a 250-mL Erlenmeyer flask, and treated with 100 mL of H O, 5 mL of 20% w/v NaOH and 5 mL of 10%
2

w/v KI. The sample is titrated with 0.1012 M AgNO , requiring 27.36 mL to reach the end point as signaled by the
3

formation of a yellow precipitate of AgI. Report the concentration of cyanide as parts per million of NaCN.

17. Before the introduction of EDTA most complexation titrations used Ag  or CN  as the titrant. The analysis for Cd , for
+ – 2+

example, was accomplished indirectly by adding an excess of KCN to form Cd(CN) , and back titrating the excess 4
2–

CN  with Ag , forming Ag(CN) . In one such analysis a 0.3000-g sample of an ore was dissolved and treated with 20.00
– +
2
–

mL of 0.5000 M KCN. The excess CN  required 13.98 mL of 0.1518 M AgNO to reach the end point. Determine the
–
3

%w/w Cd in the ore.

Enjoy. . . . . .. . . .. . . and stay safe always. . . .

EXERCISES IN SPECTROMETRY
Solve the following problems

1. Find the wave number and frequency of light with a wavelength of 700 nm 
2. A solution’s transmittance is 35.0%. What is the transmittance if you dilute 25.0 mL of the solution to 50.0 mL?
3. A solution’s transmittance is 85.0% when measured in a cell with a pathlength of 1.00 cm. What is the %T if you
increase the pathlength to 10.00 cm?
 4. The accuracy of a spectrophotometer can be evaluated by preparing a solution of 60.06 ppm K Cr O  in 0.0050 M 2 2 7

H SO , and measuring its absorbance at a wavelength of 350 nm in a cell with a pathlength of 1.00 cm. The absorbance
2 4

should be 0.640. What is the molar absorptivity of K Cr O  at this wavelength?

2 2 7

5. Dilution of a 4.95 x 10-3 M standard solution of a compound is made by taking 2.00 mL of this solution and diluting
with solvent to 25.00 mL. The diluted standard had an absorbance of 0.624 at 238 nm in a 1.00 cm cuvet. A blank
solution containing only solvent had an absorbance of 0.029 at 238 nm. The absorbance of an unknown sample of this
compound in the same solvent and cuvet had an absorbance of 0.377. What is the concentration of the compound in this
sample? What is the molar absorptivity of this compound at 238 nm?  

6. EDTA forms colored complexes with a variety of metal ions that may serve as the basis for a quantitative
spectrophotometric method of analysis. The molar absorptivities of the EDTA complexes of Cu , Co , and Ni  at three 2+ 2+ 2+

wavelengths are summarized in the following table (all values of ε are in M  cm ). –1 –1

meta
ε ε ε
l
462.9 732.0 378.7

Co 15.8 2.11 3.11

2+

Cu 2.32 95.2 7.73

2+

Ni 1.79 3.03 13.5

2+

Using this information determine the following:

(a) The concentration of Cu  in a solution that has an absorbance of 0.338 at a wavelength of 732.0 nm.
2+

(b) The concentrations of Cu  and Co  in a solution that has an absorbance of 0.453 at a wavelength of 732.0 nm and
2+ 2+

0.107 at a wavelength of 462.9 nm.

(c) The concentrations of Cu , Co , and Ni  in a sample that has an absorbance of 0.423 at a wavelength of 732.0 nm,
2+ 2+ 2+

0.184 at a wavelength of 462.9 nm, and 0.291 at a wavelength of 378.7 nm.

The pathlength, b, is 1.00 cm for all measurements.

7. The concentration of phenol in a water sample is determined by separating the phenol from non-volatile impurities by
steam distillation, followed by reacting with 4-aminoantipyrine and K Fe(CN)  at pH 7.9 to form a colored antipyrine
3 6

dye. A phenol standard with a concentration of 4.00 ppm has an absorbance of 0.424 at a wavelength of 460 nm using a
1.00 cm cell. A water sample is steam distilled and a 50.00-mL aliquot of the distillate is placed in a 100-mL
volumetric flask and diluted to volume with distilled water. The absorbance of this solution is found to be 0.394. What
is the concentration of phenol (in parts per million) in the water sample?

8. In the DPD colorimetric method for the free chlorine residual, which is reported as mg Cl /L, the oxidizing power of 2

free chlorine converts the colorless amine N,N-diethyl-p-phenylenediamine to a colored dye that absorbs strongly over
the wavelength range of 440–580 nm. Analysis of a set of calibration standards gave the following results.

mg Cl /L absorbance
2

0.00 0.000
 0.50 0.270
1.00 0.543
1.50 0.813
2.00 1.084

A sample from a public water supply is analyzed to determine the free chlorine residual, giving an absorbance of 0.113. What is
the free chlorine residual for the sample in mg Cl /L?
2

9. The concentration of the barbiturate barbital in a blood sample was determined by extracting 3.00 mL of blood with 15
mL of CHCl . The chloroform, which now contains the barbital, is extracted with 10.0 mL of 0.45 M NaOH (pH ≈ 13).
3

A 3.00-mL sample of the aqueous extract is placed in a 1.00-cm cell and an absorbance of 0.115 is measured. The pH
of the sample in the absorption cell is then adjusted to approximately 10 by adding 0.5 mL of 16% w/v NH Cl, giving
4

an absorbance of 0.023. When 3.00 mL of a standard barbital solution with a concentration of 3 mg/100 mL is taken
through the same procedure, the absorbance at pH 13 is 0.295 and the absorbance at a pH of 10 is 0.002. Report the mg
barbital/100 mL in the sample.
 
10. Jones and Thatcher developed a spectrophotometric method for analyzing analgesic tablets containing aspirin,
phenacetin, and caffeine.  The sample is dissolved in CHCl  and extracted with an aqueous solution of NaHCO  to
24
3 3

remove the aspirin. After the extraction is complete, the chloroform is transferred to a 250-mL volumetric flask and
diluted to volume with CHCl . A 2.00-mL portion of this solution is diluted to volume in a 200-mL volumetric flask
3

with CHCl . The absorbance of the final solution is measured at wavelengths of 250 nm and 275 nm, at which the
3

absorptivities, in ppm  cm , for caffeine and phenacetin are

–1 –1

a 250 a 275

0.013
caffeine 0.0485
1
0.070
phenacetin 0.0159
2

11. Aspirin is determined by neutralizing the NaHCO  in the aqueous solution and extracting the aspirin into CHCl . The
3 3

combined extracts are diluted to 500 mL in a volumetric flask. A 20.00-mL portion of the solution is placed in a 100-
mL volumetric flask and diluted to volume with CHCl . The absorbance of this solution is measured at 277 nm, where
3

the absorptivity of aspirin is 0.00682 ppm  cm . An analgesic tablet treated by this procedure is found to have
–1 –1

absorbances of 0.466 at 250 nm, 0.164 at 275 nm, and 0.600 at 277 nm when using a cell with a 1.00 cm pathlength.
Report the milligrams of aspirin, caffeine, and phenacetin in the analgesic tablet.
 
 
 
 
 
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Exercise in Gravimetric Analysis

Solve the following problems

1. A sample containing 18.0% of Fe O is treated and analyzed forming a precipitate  of Fe O . If the

3 4 2 3

weight of the precipitate is 0.100 g. What is the weight of the sample needed for the analysis?
2. The calcium from a sample of limestone weighing 607.4 mg was precipitated as calcium oxalate CaC2O4
and ignited to calcium carbonate CaCO3 weighing 246.7 mg. What is the mass of calcium in the sample?

3. A commercial algaecide containing an organocopper compound was treated with nitric acid and
evaporated  to dryness. After dissolution of the residue, the copper was precipitated with alpha-benzoine
oxime. If the sample weighed 15.443 g and the precipitate of Cu(C14H12NO2)2 weighed 0.6314, . what is
the % Cu in the sample?

4. An organic pesticide (MW 183.7) contains 8.43% Cl. A 0.627-g sample containing the pesticide plus
inert material containing no chloride was decomposed with metallic sodium in alcohol.  The liberated
chloride ion was precipitated as AgCl weighing 0.0831 g.  Calculate the percentage of pesticide in the
sample.

5. The nitrogen content of a 3.6342 g sample of undried spinach leaves was determined to be 4.63 % and the
moisture content is  was 8.68 %. What is the % of nitrogen in the dried sample?

6. The concentration of arsenic in an insecticide is determined gravimetrically by precipitating

MgNH4AsO4 and isolating Mg2As2O7. Determine the %w/w As2O3 in a 1.627-g sample of
insecticide if it yields 106.5 mg of Mg2As2O7.

7. A 516.7-mg sample containing a mixture of K2SO4 and (NH4)2SO4 was dissolved in water and
treated with BaCl2, precipitating the SO as BaSO4. The resulting precipitate was isolated by
4
2–

filtration, rinsed free of impurities, and dried to a constant weight, yielding 863.5 mg of BaSO4. What
is the %w/w K2SO4 in the sample? 

8. The amount of iron and manganese in an alloy can be determined by precipitating the metals with 8-
hydroxyquinoline, C9H7NO. After weighing the mixed precipitate, the precipitate is dissolved and the
amount of 8-hydroxyquinoline determined by another method. In a typical analysis a 127.3-mg sample
of an alloy containing iron, manganese, and other metals was dissolved in acid and treated with
appropriate masking agents to prevent an interference from other metals. The iron and manganese
were precipitated and isolated as Fe(C9H6NO)3 and Mn(C9H6NO)2, yielding a total mass of 867.8
mg. The amount of 8-hydroxyquinolate in the mixed precipitate was determined to be 5.276 mmol.
Calculate the %w/w Fe and %w/w Mn in the alloy.

9. A 0.8612-g sample of a mixture of NaBr, NaI, and NaNO3 was analyzed by adding AgNO3 and
precipitating a 1.0186-g mixture of AgBr and AgI. The precipitate was then heated in a stream of Cl2,
converting it to 0.7125 g of AgCl. Calculate the %w/w NaNO3 in the sample.

10. The earliest determinations of elemental atomic weights were accomplished gravimetrically. In
determining the atomic weight of manganese, a carefully purified sample of MnBr2 weighing 7.16539
g was dissolved and the Br– precipitated as AgBr, yielding 12.53112 g. What is the atomic weight for
Mn if the atomic weights for Ag and Br are taken to be 107.868 and 79.904, respectively?
11.  A sample of impure pyrite known to be approximately 90% w/w FeS2 is to be analyzed by oxidizing
the sulfur to SO4 and precipitating it as BaSO4. How many grams of the sample must you take to
2–

form at least 1 g of BaSO4?

12. Calcium is determined gravimetrically by precipitating CaC2O4•H2O and isolating CaCO3. After
dissolving a sample in 10 mL of water and 15 mL of 6 M HCl, the resulting solution is heated to
boiling and a warm solution of excess ammonium oxalate is added. The solution is maintained at 80
oC and 6 M NH3 is added dropwise, with stirring, until the solution is faintly alkaline. The resulting
precipitate and solution are removed from the heat and allowed to stand for at least one hour. After
testing the solution for completeness of precipitation, the sample is filtered, rinsed with 0.1% w/v
ammonium oxalate, and dried at 100–120 oC for 1 hour. The precipitate is transferred to a muffle
furnace where it is converted to CaCO3 by drying at 500 ± 25 oC until constant weight. Why is the
precipitate of CaC2O4•H2O converted to CaCO3? In the final step, if the sample is heated at too high
of a temperature some CaCO3 may be converted to CaO. What effect would this have on the reported
%w/w Ca? 

13. To determine the amount of iron in a dietary supplement, a random sample of 15 tablets weighing a
total of 20.505 g was ground into a fine powder. A 3.116-g sample was dissolved and treated to
precipitate the iron as Fe(OH)3. The precipitate was collected, rinsed, and ignited to a constant weight
as Fe2O3, yielding 0.355 g. Report the iron content of the dietary supplement as g FeSO4•7H2O per
tablet. 

14. After preparing a sample of alum, K2SO4•Al2(SO4)3•24H2O, a student determined its purity by
dissolving a 1.2391-g sample and precipitating the aluminum as Al(OH)3. After filtering, rinsing, and
igniting, 0.1357 g of Al2O3 is obtained. What is the purity of the alum preparation?

15. The number of ethoxy groups (CH3CH2O–) in an organic compound is determined by the following
two reactions.
R(CH2CH3)x   +  xHI      ==== R(OH)x   +  xCH3CH2I
CH3CH2I   + Ag  +  H2O   ==== AgI  + CH3CH2OH 

A 36.92-mg sample of an organic compound with an approximate molecular weight of

176 was treated in this fashion, yielding 0.1478 g of AgI. How many ethoxy groups are there in
each molecule of the compound?

16. A sample containing BaCl .2H O, KCl and inert material weighs 0.8417g. This sample was heated to
2 2

160 C for 45 minutes to remove the water in the sample. After heating, it weighs 0.8076 g. The
o

sample was then dissolved in water and treated with slight excess of AgNO . The resulting precipitate
3

was collected and found to weigh 0.5847. Calculate the BaCl .2H O and % KCl in the sample.
2 2

17. A 0.4800-g sample that contains KCl, KI and inert material gives a precipitate of AgCl and AgI that
weighs 0.2720 g. A 0.7200-g sample of the same material completely reacted with 25.80 ml of 0.1020
M AgNO . Calculate the percent KCl and KI in the sample.
3

18. A 0.9250 g sample containing sodium and potassium is treated with chlorides to form NaCl and KCl
salts.  The chloride mixture weighs 0.6065 g. The chlorides are then treated with sulfates to form
 Na SO . and  K SO and the mixture weights 0.7190 u. What is the percent composition of Na and K in
2 4 2 4 

the sample?

19. The iron in an organometallic compound was determined by treating a 0.4873-g sample with HNO3
and heating to volatilize the organic material. After ignition, the residue of Fe2O3 weighed 0.2091 g. 

a. What is the %w/w Fe in this compound? 

b. The carbon and hydrogen in a second sample of the compound were determined by a combustion
analysis. When a 0.5123-g sample was carried through the analysis, 1.2119 g of CO2 and 0.2482 g of
H2O were collected. What are the %w/w C and %w/w H in this compound and what is the
compound’s empirical formula?

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