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8 views

Lec 5

Uploaded by

bifusk481
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Al-Esra’a University College

Department of Pharmacy

An Introduction to Gravimetric Analysis

Prof. Dr.
A. M. AL. Haideri
First Stage – Term 1
Inorganic and organic precipitating
agents gravimetric factors and scope
of applications
Gravimetric methods of analysis
 In gravimetric analysis, the mass of a product is used to calculate the
quantity of the original analyte.
 The gravimetric methods of analysis are based on mass measurement
made with an analytical balance.
 a Several analytical methods are based on mass measurement :
1. Precipitation gravimetry.
2. Volatilization gravimetry.
3. Electro gravimetry.
4. Gravimetric titrimetry.
5. Atomic mass spectrometry.
Precipitation Gravimetry:
In this analytical method , the analyte is converted to a sparingly
soluble precipitate. This precipitate is then filtered, washed free of
impurities, converted to a product of known composition by
suitable heat treatment, and weighed. A familiar example of
gravimetric (precipitation) analysis is the determination of CI⁻ by
precipitation with Ag⁺
Ag⁺ + Cl⁻ AgCl(s)
The weight of AgCl produced tells us how much CI⁻ was originally
present according to the stoichiometry of the reaction.
Stoichiometry is the calculation of quantities of substances
involved in chemical reaction, for example each mol of Fe2O3 has 2
mol Fe (Fe2O3 2Fe).
The following terms are used in this chapter:
Precipitation: process in which the analyte is converted to sparingly
soluble product (i.e precipitate)
Precipitate: the product of the process.
Precipitant: the agent that cause precipitation. the precipitant or
(precipitating agent) should react specifically (which it reacts only with
a single species an example is dimethyl-glyoxime which precipitates
only Ni+2 from alkaline solution.
Another type of precipitants are selective reagents, which are more
common react with a limited number of species. An example of
selective reagent is AgNO3 the only common ions that precipitate from
acidic solution are CI⁻, Br⁻, I⁻ and SCN⁻.
Features of the ideal precipitate:

The ideal product (precipitate) of a gravimetric analysis should be


1. Insoluble that no significant loss of the analyte occurs during filtration and
washing.
2. Easily filtered and washed free of contaminants.
3. Posses a known composition after it is dried, or if necessary ignited.
4. Very pure and unreactive with constituents of the atmosphere
5. The particles should not be small that they clog or pass through the filter
paper.
Some important organic precipitants

Name Structure Ions precipitated

Dimethylglyoxime 𝑁𝑖 +2 , 𝑃𝑑 +2 , 𝑃𝑡 +2

𝑀𝑔+2 , 𝑍𝑛+2 , 𝐶𝑢+2 , 𝐶𝑑+2 , 𝑃𝑏+2 ,


𝐴𝑙 +3 , 𝐹𝑒 +3 , 𝐵𝑖 +3 , 𝐺𝑎+3 , 𝑇ℎ+4 ,
8-hydroxyquinoline 𝑍𝑟 +4 , 𝑈𝑂2+2 , 𝑇𝑖𝑜 +2
8-hydroxyquinoline

Dimethylglyoxime
Some important inorganic precipitants

Species analyzed Precipitated form Form weighed


𝐵𝑎+2 𝐵𝑎𝑆𝑂4 𝐵𝑎𝑆𝑂4
𝑃𝑏 +2 𝑃𝑏𝑆𝑂4 𝑃𝑏𝑆𝑂4
𝐴𝑔+1 𝐴𝑔𝐶𝑙 𝐴𝑔𝐶𝑙

Crystallization occurs in two phases: nucleation and particle growth.


Gravimetric calculations
A gravimetric analysis required two experimental measurement:
1) The weight of sample taken
2) The weight of product of known composition determined from the sample
Ordinarily these data are converted to percentage of analyte by a simple
mathematical manipulation
𝒘𝒕. 𝒂𝒏𝒂𝒍𝒚𝒕𝒆
% 𝒂𝒏𝒂𝒍𝒚𝒕𝒆 = × 𝟏𝟎𝟎
𝒘𝒕. 𝒔𝒂𝒎𝒑𝒍𝒆
The stoichiometric equation is used to calculate the wt. of analyte present in
the precipitate using the gravimetric factor.
Gravimetric factor (G.F): is needed to convert the weight of the precipitate
to the corresponding weight of analyte.
𝒘𝒕. 𝒂𝒏𝒂𝒍𝒚𝒕𝒆 = 𝒘𝒕. 𝒑𝒓𝒆𝒄𝒊𝒑𝒊𝒕𝒂𝒕𝒆 × 𝑮. 𝑭

𝒈. 𝑭𝒘𝒕. 𝒂𝒏𝒂𝒍𝒚𝒕𝒆 𝒂
𝑮. 𝑭 = ×
𝒈. 𝑭𝒘𝒕. 𝒐𝒇 𝒑𝒓𝒆𝒄𝒊𝒑𝒊𝒕𝒂𝒕𝒆 𝒃
Where:
a= number of mole of analyte (sought) from the stoichiometric relation.
b= number of mole of precipitate (sought) from the stoichiometric relation.
Example1: how many gram of cl (Fwt.=35.45)
are contained in a precipitate of AgCl
(Fwt.=143.3) that weighs 0.204 gram.

Ag⁺(aq)+Cl⁻ AgCl (ppt)

𝒘𝒕. 𝒂𝒏𝒂𝒍𝒚𝒕𝒆 = 𝒘𝒕. 𝒑𝒓𝒆𝒄𝒊𝒑𝒊𝒕𝒂𝒕𝒆 × 𝑮. 𝑭


𝒈. 𝑭𝒘𝒕 𝒄𝒍 𝟏
𝒘𝒕. 𝑪𝒍 = 𝒘𝒕 𝑨𝒈𝑪𝒍 × ×
𝒈. 𝒇𝒘𝒕. 𝑨𝒈𝑪𝒍 𝟏
𝟑𝟓. 𝟒𝟓
𝒘𝒕. 𝑪𝒍 = 𝟎. 𝟐𝟎𝟒 × = 𝟎. 𝟎𝟓𝟎𝟓𝒈
𝟏𝟒𝟑. 𝟑𝟏
Example 2: to what weight of AgCl3
(Fwt.=133.3) would 0.204 g of AgCl
correspond?

The stoichiometric relation AgCl= 3 AgCl


Ag⁺+3Cl⁻ AgCl3
Ag⁺ + Cl⁻ AgCl(ppt)
𝒈. 𝑭𝒘𝒕 𝑨𝒍𝑪𝒍𝟑 𝒂
𝒘𝒕. 𝑨𝒍𝑪𝒍𝟑 = 𝟎. 𝟐𝟎𝟒 𝒈 𝑨𝒈𝑪𝒍 × ×
𝒈. 𝒇𝒘𝒕. 𝑨𝒈𝑪𝒍 (𝒑𝒑𝒕) 𝒃
𝟏𝟑𝟑. 𝟑 𝟏
= 𝟎. 𝟐𝟎𝟒 × × = 𝟎. 𝟎𝟔𝟔𝒈 solution
𝟏𝟒𝟑. 𝟑𝟏 𝟑
Example 3: the calcium in a 200 mL sample of a natural water was determined by
precipitating the cation (Ca⁺⁺) as CaC2O4. the ppt was filtered, washed and ignited
in a crucible with an empty mass of 26.6002g. The of the crucible plus CaO (Fwt
56.077 g/mol) was 26.7134 g. calculate the conc. Of Ca (Fwt 40.078 g/mol) in
water in units of grams per 100 mL of water.

Solution: the mass of CaO is


26.7134-26.6002=0.1132 g
+
𝑔 𝐹𝑤𝑡. 𝐶𝑎 (𝑎𝑛𝑎𝑙𝑦𝑡𝑒) 𝑎
𝑤𝑡. 𝑜𝑓 𝐶𝑎 = 𝑤𝑡. 𝐶𝑎𝑂 × ×
𝑔 𝐹𝑤𝑡. 𝐶𝑎𝑂 (𝑝𝑝𝑡) 𝑏
Ca++ CaO
40.078 1 0.0809 𝑔 𝐶𝑎⁺
𝑤𝑡. 𝑜𝑓 𝐶𝑎+= 0.1132 × × =
56.077 1 200𝑚𝐿
+
0.04045 𝑔
𝐶𝑎 𝑖𝑛 100 𝑚𝐿 = 𝑤𝑎𝑡𝑒𝑟
100 𝑚𝐿
Example 4: an iron ore was analyzed by dissolving a 1.1324 g
sample in conc. HCl. The resulting solution was diluted with water
and the iron (III) was precipitated as the hydrous oxide Fe2O3.Xh2o
by the addition of NH3 after filtration and washing. The residue was
ignited at a high temperature to give 0.5394 g of pure Fe2O3 (159.69
g/mol). Calculate
(a) the % Fe (55.847 g/mol)
(b) the % Fe3O4 (231.54 g/mol) in the sample.
Example 5: A 0.2356 g sample containing only NaCl
(58.44 g/mol) and BaCl2 (208.23 g/mol) yielded 0.4637 g of
dried AgCl (143.32 g/mol). Calculate the percent of each
halogen compound in sample.

Try to solve it
Questions & problems
(1) List the major steps commonly involved in a gravimetric
determination.
(2) What is a gravimetric factor?
(3) What weight of Ag (At.mass=107.87) is present in 100.0g of AgCl
(F.wt=143.32). Ans.=75.27g
(4) What amount of NaCl (F.wt=58.44) is present in a sample that yields
on precipitation of chloride with AgNO3 0.8342 g of AgCl
(F.wt=143.32). Ans.=0.3402
(5) How much BaCl2 (F.wt=208.24) is present in a solution if on addition
of a sufficient amount of AgNO3, the weight of isolated AgCl
(F.wt=143.32) is 1.3456 g? Ans.=0.9776g
Try to solve it
and good luck

(6) A mixture of NaCl (F.wt=58.44) and Na2SO4 is to be analyzed for its


NaCl content. A sample weighing 0.9532 is dissolved in water and the
chloride precipitated by the addition of an excess of AgNO3. the dried
precipitate of AgCl (F.wt=143.32) weighs 0.7033 g. what is the percent
NaCl in the sample? Ans.=30.09%
(7) Sodium tetraphenylborate NaB(C6H5)4 is used as precipitant for
potassium. What is the w/w% of K2O (F.wt=94.20) in a fertilizer when a
0.4320 g sample gives 0.2138 g of K2B(C6H5)4 (F.wt=358.2).
Ans.=???
Thankyou for
listening

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