Document Type

Prepared by

Work Instruction

Laboratory Superintendent

Approved by

Effective Date

Quality Manager

1 January 2015

Next Review Da
Signed

Signed

01 January 2016

1. PURPOSE AND SCOPE

1.1. This work instruction covers the reference method for free lime analysis using
the complexometry method.
2. REFERENCE
None
3. DEFINITIONS
None
4. RESPONSIBILITY
The Works Chemist is responsible for the proper implementation and revision of
this procedure
5. SAFETY
5.1. Wear lab coats whenever working with chemicals
5.2. Wear safety glasses when handling chemicals
5.3. Wear gloves whenever working with harsh chemicals
5.4. Inspect and discard any broken glassware (collect it using the appropriate
container made for this purpose)
5.5. Work under a functional fume hood.
5.6. Always refer to the Material Safety Data Sheets (MSDS)

5.7. Identify all containers used as reagents

Document Number

Title

Revision Number

Page Number

M/LAB/WI 0009

Determination of Free Lime by

2 of 4

Document Type

complexometry method
Prepared by

Work Instruction

Laboratory Superintendent

Approved by

Effective Date

Quality Manager

1 January 2015

Next Review Da
Signed

Signed

6. APPARATUS AND MATERIALS

6.1. Drying oven at 110C 5C.
6.2. Vacuum filtration assembly
6.3. 100ml and 600ml beakers, watch glass and 500ml flask.
6.4. 18l polyethylene container.
6.5. 10 and 50-mL volume burette with a minimum precision of 0.1mL.
6.6. White surface with light to improve colour change detection (end-point).
6.7. Indicator papers: working range pH 9.5 to 13. (a pH meter is not necessary).
6.8. Magnetic stirrer with bar magnets.
6.9. Precision balance ( 1mg).
7. REAGANTS
7.1. Ethylene glycol 99.5% at least, with 0.1% max of water.
7.2. HCl 1+1 solution
7.3. Ammonia 28 % Normapur.
7.4. Patton & Reeders reagent
7.5. Sodium Hydroxide 2N solution
7.6. Commercial standardised solution EDTA
7.7. Deionised water
7.8. Methyl orange 0.1%
7.9. Ethyl alcohol (Maximum 0.05% of water)
7.10.

Triethanolamine (TEA) Solution 1+2

7.11.

Phtaleine purple indicator

7.12.

Most recent IU annual cement for repeatability test only.

01 January 2016

Document Number

Title

Revision Number

Page Number

M/LAB/WI 0009

Determination of Free Lime by

3 of 4

Document Type

complexometry method
Prepared by

Work Instruction

Laboratory Superintendent

Approved by

Effective Date

Quality Manager

1 January 2015

Next Review Da
Signed

Signed

01 January 2016

8. METHOD
8.1. Weigh 2.00+/-0.01g of sample
8.2. Add 25ml of ethylene glycol into a dry 100ml beaker
8.3. Add the sample to the solution
8.4. Mix with a magnetic stirrer for 30sec
8.5. Place the beaker in an oven at 110oC for 10mins
8.6. Take out the beaker. Stir with magnetic stirrer for 30sec
8.7. Return the beaker to the oven for another 10mins
8.8. Take out the beaker. Stir with a magnetic stirrer for 30sec
8.9. Place a new filter
8.10.

Wet the filter with ethyl alcohol

8.11.

In the vacuum device

Add 200ml of deionised water

Add 5ml of HCl 1+1

Add 5 drops of methyl orange indicator

8.12.

Filter the sample with the vacuum filtering device

8.13.

Rinse the beaker and magnetic stirrer with ethyl alcohol (3 washings) to

collect all dissolved free lime

8.14.

Before titration add the following to the filtrate

4ml of ammonia 28%

15ml of triethanolamine

A scoop (20mg) of Patton & Reeders

Slowly add NaOH 2N until it turns pink. Add drops of NaOH until pH level
reaches 13+/-0.5

Document Number

Title

Revision Number

Page Number

M/LAB/WI 0009

Determination of Free Lime by

4 of 4

Document Type

complexometry method
Prepared by

Work Instruction

Laboratory Superintendent

Approved by
Quality Manager

Effective Date
1 January 2015

Next Review Da
Signed

8.15.

Signed

01 January 2016

Start the magnetic stirrer and deliver a stream of EDTA. As you

approach the endpoint (when colour changes from pink to a stable torquoise
blue), titrate at a slower speed (in drops)
8.16.

Record the amount of EDTA added (in ml)

8.17.

Calculate the free lime in the sample as follows:

% fCaO

CC EDTA V EDTA 56.08 100

Wsample 1000

%fCaO

= percentage of free lime in the sample

CCEDTA

=EDTA concerntration (mol/L)

VEDTA

=ml of EDTA added

Wsample

=weight of sample in g

56.8

=molecular weight of CaO in g/mol

56.9

=1000ml/l

9. RECORDS
Labdatase YR/Month-LQTS-Free lime monitoring file