Tutorial 4: ANSWER SCHEME

1. Define sampling and explain the purpose of sampling:

SAMPLING is a process to get a representative and homogeneous sample to produce

meaningful information.

PURPOSE OF SAMPLING is to obtain a representative samples of the whole sample

that can be taken to the laboratory for chemical analysis and the results obtain will be
accurate.

2. Describe a sampling technique for solid sample.

 To collect a solid sample, coning and quartering method is used.

a. Divide a pile of material into quarter and take a sample from each quarter of the pile
and crush these samples to a smaller conical pile.
b. Flatten the conical pile and cut into equal quarters.
c. Two opposite quarters are chosen at random.
d. Then, crush the quarter further.
e. The whole steps are repeated until a laboratory samples obtain.

3. Briefly describe the ‘wet digestion’ techniques and give two examples of reagent used in
this technique.
Wet Digestion Techniques
 A method use to decompose or eliminate an organic material by treatment with
strong liquid oxidizing agents or mixture of acids. The acids oxidize organic
matter to CO2, H2O and other volatile products, which are driven off, leaving
behind inorganic constituents without losing element to be determined.
 PROCESS:
 The technique will performed in Kjedahl flask, and undergo in a fume hood.
 The sample will treat with acid digestion to achieve a complete dissolution.
(mixture of H2SO4 (small amount) and HNO3,(large amount) )
 HNO3 will destroys the bulk of organic matter, but not destroy the last traces.
 During acid digestion process, the solution is boiled off and white SO3 fumes
evolve, until H2SO4 remains and dense and destroy the remaining organic matter.
 The digestion is continued until producing clear solution.
 Reagent used: Mixture of H2SO4 and HNO3 or mixture of HCl and HNO3
4. Give two examples of primary standard and list the properties of primary standard.
 Na2CO3 solution (Sodium carbonate)
 KHC8H4O4 solution (Potassium hydrogen phthalate)

Properties of primary standard solution

o must exhibit HIGH PURITY, typically 100 ± 0.05 %.
o must exhibit HIGH STABILITy, must be stable with respect to both spontaneous
decomposition and reaction with moisture.
o should not contain water of hydration
o High equivalent weight (more stable) to standardize the solution
o must not be costly.
o easily available.
o must be readily soluble

5. If a water sample is to be analyzed for trace levels of metals, briefly explain why a
glass container for sampling and storage is inappropriate.
 Metal will undergo retention on a glass container
 Metal will react with the vessel or walls of the glass container, this will cause
contamination of the sample and loss of analytes that want to be analyzed

6. Explain briefly the preparation of 250 mL 10% (w/v) of Ca (NO3)2 in the laboratory.

10% = weight of solute (g) / volume solution (mL) x 100

10 g/mL x 250 mL = 25 g Ca(NO3)2

100

How to prepare: Weigh accurately 25 g Ca(NO3)2, dissolve in small amount of distilled

water, transfer to a 250 mL volumetric flask and dilute with distilled water to the mark.
7. List advantages and disadvantages of wet digestion and dry ashing.
WET ASHING DRY ASHING
ADVANTAGES DISADVANTAGES ADVANTAGES DISADVANTAGES
Superior in term of Introduction of Simpilicity, safe -Losses due to
rapidity impurities from the retention to the ashing
reagent necessary container or walls of
for the reaction the vessel
-Losses due to
volatilazation of
elements
Freedom from loss Free from 2-4 hour are needed
by contaminations for dry ashing
retention since few or no
reagents are
added
Low level of Adsorbed metals on
temperature the vessel may in turn
maintained contaminate future
samples

8. An analyst wants to know the level of pesticide residue on the leaves of tobacco plants
grown in 100 m2 plot of land. Describe the correct sampling procedure that should be
carried out.
 Obtain the representative sample of the leaves of tobacco plants grown in 100 m2
plot of land
 Take a gross sample of the leaves of tobacco plant by taking 1/50 to 1/100 of the
total leaves of tobacco plant in a 100 m2 plot of land
 Reduce the gross sample until obtain laboratory samples by using coning and
quartering method

9. A river water samples was collected a week before it was analyzed for a trace level of
metals. Discuss the problem encountered during storage of the sample and ways to
overcome the problem.
Problems:
 Loss of water from hygroscopic material
 Loss of volatile analytes from water samples
 Precipitation of metals from water sample
 Decomposition of sample
 Sample can be contaminated by foreign matter
 Side chain reaction and reaction of sample between wall of container occurred
may change the properties of sample
 To overcome:
 The sample kept in bottles with stoppers
 The bottles or container should be clean and free from impurities
 Avoid using glass container

10. Primary standard sodium carbonate solutions containing 0.25 g of Na2CO3 required
30.50 mL of hydrochloric acid solution for standardization of HCl. Identify the titrant and
primary standard and then calculate the molarity of the HCl solution. (molar mass
Na2CO3 = 106 g/mol)
Titrant: HCl, Primary standard: Na2CO3
Balance equation: Na2CO3 + 2HCl  2NaCl + CO2 + H2O

Mol Na2CO3 = 0.25g /106 g/mol = 2.3585 x 10-3 mol

1 mol Na2CO3 ≈ 2 mol HCl
2.3585 x 10-3 mol Na2CO3 x 2 mol HCl = 4.717 x 10-3 mol HCl
1 mol Na2CO3
Molarity HCl = Mol/L
= 4.717 x 10-3 mol HCl/ 30.5 x 10-3 L = 0.155 M