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Volumetric Analysis

Introduction The Equipment The Process Calculations

Author: J R Reid

Introduction
Analisis volumetri merupakan teknik penetapan jumlah sampel melalui perhitungan volume
Bahan bahan yang diperlukan: Zat yang diketahui konsentrasinya yang akan bereaksi dengan senyawa yang akan dicari konsentrasinya (unknown) Indikator yang akan menunjukkan kapan reaksi selesai Alat alat yang dapat mengukur volume secara akurat.

The Equipment
Alat yang dibutuhkan:
Pipette/pipet mengukur larutan secara tepat (pipet volume/ukur, pipet gondok)
Burette/buret meneteskan sejumlah reagen cair dalam eksperimen yang memerlukan presisi, seperti pada eksperimen titrasi Conical flask/ erlenmeyer mencampurkan larutan Funnel/corong membantu memasukkan cairan kedalam wadah yang memiliki lubang sempit agar tidak tumpah

Wash bottles/botol semprot berisi air suling untuk membersihkan peralatan


Volumetric flasks/labu takar mengencerkan atau membuat larutan dengan volume tertentu secara akurat.

The Process - Preparation


Two solutions are used:
The solution of unknown concentration; The solution of known concentration this is also known as the standard solution

Write a balanced equation for the reaction between your two chemicals Clean all glassware to be used with distilled water. The pipettes and burettes will be rinsed with the solutions you are adding to them

Buret dijepit pada clamp stand di atas erlenmeyer Buret diisi larutan (misalnya larutan standar)

Pipet untuk memindahkan larutan ke erlenmeyer


Tambahkan indikator ke erlenmeyer

Process The Titration


Baca volume awal larutan dalam buret Buka kran untuk memulai reaksi ke dalam erlenmeyer, goyang erlenmeyer secara kontinyu. Pada saat indikator mulai berubah warna, kecepatan aliran buret mulai diperlambat. Ketika perubahan warna permanen, hentikan aliran dan baca volume akhirnya. Volume total yang dioerlukan disebut titer. Ulangi titrasi, karena anda telah mengetahui volume sebelumnya, maka anda dapat mengulanginya dengan lebih tepat.

Calculations Mean Titre


We will have a number of titres for each solution we analysed. The first thing we do is to calculate the mean (average) titre:
Titres Mean = 12.6 ml 13.0 ml 13.1 ml 12.9ml = Sum of the titres / number of titres = (13.0 + 13.1 + 12.9) / 3 = 13.0ml

Why did we discard the 12.6 ml reading?

Calculations The Unknown Concentration Preparation


1.
2.

Write down the balanced equation e.g.


H2SO4 + 2NaOH Na2SO4 + 2H2O

Write down everything else we know. This will be:


a. b. c. d.

Volume of liquid in the pipette Mean titre (from burette) The concentration of the standard solution Was the standard solution in the pipette or in the burette?

Calculations The Unknown Amount


3.

4.

Now calculate the amount in the standard solution you used. Use the n = cv formula. Remember: the millilitres must always be converted into litres for these formulae Now that you know how many moles of the standard you used, look at the balanced equation. Would you need more or less of the unknown substance in a balanced reaction?
If more, then how much more two times, three times? If less, then how much less half as much, one third?

We can calculate the amount of the unknown:


We multiply if we need more i.e. 2x, 3x, etc We divide if we need less i.e. = divide by 2, etc

Calculations The Unknown Concentration


5.

Now we have the volume and amount of the unknown substance. We can now rearrange our n = cv formula to say c = n/v
Remember:
All the calculations must be in litres (not millilitres) The final value must have units (molL-1) written after it

Example:
1. 2.

H2SO4 + 2NaOH Na2SO4 + 2H2O Standard solution = NaOH (in burette) = 0.1molL-1 Unknown concentration = H2SO4 (from 20ml pipette) Titres = 12.6ml, 13.1ml, 13.0, 12.9ml Average titre = (13.1+13.0+12.9) / 3 = 13.0ml

3. 4. 5.

Amount of NaOH = cv = 0.1 x (13/1000) = 0.0013mol Amount of H2SO4 = half of NaOH = 0.0013/2 = 0.00065mol Concentration H2SO4 = n/v = 0.00065/(20/1000) = 0.325molL-1

Titration examples A
HCl + NaOH NaCl + H2O
Titres: 12.1mL, 12.3mL, 12.1mL, 12.0mL Known solution details: HCl in the burette, Concentration = 0.522 molL-1 Unknown solution details: NaOH 15mL aliquots Calculations:

Titration examples B
CH3COOH + NaOH NaCH3COO + H2O
Titres: 17.6mL, 18.5mL, 17.4mL, 17.5mL Known solution details: NaOH in the burette, Concentration = 0.103 molL-1 Unknown solution details: CH3COOH 15mL aliquots Calculations:

Titration examples C
2HCl + Na2CO3 2NaCl + H2O + CO2
Titres: 12.8mL, 12.8mL, 12.8mL, 12.9mL Known solution details: HCl in the burette, Concentration = 0.555 molL-1 Unknown solution details: Na2CO3 25mL aliquots Calculations:

Titration examples D
H2SO4 + 2NaOH Na2SO4 + 2H2O
Titres: 12.1mL, 12.3mL, 12.1mL, 12.0mL Known solution details: NaOH in the burette, Concentration = 1.04 molL-1 Unknown solution details: H2SO4 10mL aliquots Calculations:

Level 3 Spot the difference


Here is an extract from a level 3 titration assessment. It shows an example of a chemical reaction that could be used in a titration:
Hypochlorite ions react with iodide ions according to the equation; OCl + 2I+ 2H+ Cl + I2 + H2O

The iodine produced is then titrated with standardised sodium thiosulfate solution. It reacts according to the equation below. I2 + 2S2O32 2I + S4O62

Since starch turns blue in the presence of iodine, it is used as an indicator for this final reaction.
The overall equation for both reactions is: OCl + 2H+ + 2S2O32 Cl + S4O62 + H2O