Final Q.C MANUAL
Final Q.C MANUAL
Final Q.C MANUAL
MANUAL
for EDIBLE SALT manufacturing
Forward
Consequent upon the resolution, dated April 30th, 2019 passed by the board
of Directors of the company " Himalayan Edibles Private Limited" Pakistan in its meeting held on
April 30th, 2019 at Lahore, it was resolved that company being engaged in manufacturing edible salt
must introduce a laboratory manual for observing standard testing procedures in the laboratory
established at manufacturing plant site. These standard testing procedures shall be followed strictly
by the lab attendants while performing quality control tests of iodine fortified salt.
1. Salt reduction and iodine fortification strategies in public health. (March 2013)
2. Sodium intake for adults and children. Geneva, World Health Organization
(WHO), 2012. (Reprinted in 2014)
3. Potassium intake for adults and children Geneva, World Health Organization
(WHO), 2012. (Reprinted in 2014)
TABLE OF CONTENTS
1 DEFINITIONS
Rock Salt Natural form of Salt mined from Salt mines also called Halite.
Fortification Fortification is the practice of deliberately increasing the content
of an essential micronutrient, i.e. vitamins and minerals
including trace elements in a food to improve the nutritional
quality and provide a public health benefit.
ppm This is an abbreviation for "parts per million"
It is also can be expressed as milligrams per liter (mg/L) or
mass of a chemical or contaminate in mg / kg.
density Density, mass of a unit volume of a material substance.
density = d = M/V, (M is mass, and V is volume.)
Expressed as units of grams per cubic centimeter.
Density describes how compact or concentrated something is
Solubility Solubility is the property of a solid, liquid or gaseous chemical
substance called solute to dissolve in a solid, liquid or gaseous
solvent. The resulting solution is called a saturated solution.
mesh one of the openings between the threads or cords of a net. often
used to designate screen size as the number of openings per
linear inch.
Crystal A crystal consists of substance that is formed from an ordered
arrangement of atoms, molecules, or ions. there are repeated
units, crystals have recognizable structures well-defined angles
and faces.
sodium chloride Salt is the main mineral constituent of sea water. The concentration of
salt in sea water as about 35 grams (1.2 oz) of solids per liter of sea water.
Salt occurs in the form of an irregular dome like structure. There are seven thick salt
seams with cumulative thickness of about 150 meters. At places rock salt is 99% pure.
Salt is transparent, white, pink, reddish to beef red color.
( iii ) STRUCTURE
Rock salt forms in crystals with a simple cubic symmetry. When it is broken, it
will break evenly into cubes and when it shatters, the pieces will be of different
sizes and shapes.
( iv ) COMPRESSIVE STRENGTH:
The unconfined compressive strength of rock salt is 21.58 MPa. or 3129.9144 Psi
Changes of the compressive strengths are fairly minor when increasing the
confining pressure from 15 MPa to 40 MPa.
1. VISUAL APPEARANCE:
The Salt should be white crystalline substance, free from any visible impurities
and harmful / toxic substances.
2. PURITY:
Sodium Chloride content (as NaCl) percent by mass shall be Min. 98%.
4. MOISTURE CONTENTS:
The salt shall not contain more than 3.0 percent by mass of moisture.
Moisture contents shall evaluated using standard method prescribed in
PS:ISO:2483 – 1973 for Determination of loss of mass at 110º C.
Dried in accordance with the method prescribed in PS : 3746 – 1996
5. PARTICLE SIZE:
99% of the salt material shall preferably pass through 1.00 mm PS: Sieve.
6. IODINE CONTENT:
Iodine contents at manufacturing stage shall not be lower than 30 ppm
Potassium Iodate (KIO3) shall not be lower than 50 ppm on dry weight
basis with one year of manufacture.
Iodine contents at distribution channel and at retail level 15 to 25 parts per
million on dry weight basis.
7. FOOD ADDITIVES:
Food additives listed in tables 1 & 2 of the Codex General Standard for Food
additives (CODEX STAN 1-192-1995) in Food Category 12.1.1 (Salt) may be used
in foods subject to this standard.
8. CONTAMINANTS:
Iodized Food Grade Salt shall not contain contaminants in amounts and in such
form that may be harmful to the health of the consumer. In particular the
following maximum limits shall not be exceeded.
9. ARSENIC:
Not more than 0.5 mg/kg expressed as As.
10. COPPER:
Not more than 2.0 mg/kg expressed as Cu.
11. LEAD:
Not more than 2.0 mg/kg expressed as Pb.
12. CADMIUM:
Not more than 0.5 mg/kg expressed as Cd.
13. MERCURY:
Not more than 0.1 mg/kg expressed as Hg.
14. HYGIENE:
In order to ensure that proper standards of food hygiene are maintained until the
product reaches the consumer, the method of production, packing, storage and
transportation of Iodized Food Grade Salt shall be such as to avoid any risk of
contamination.
CODEX STAN 192-1995, Ref: Table 1 & 2, page # 406/480 may be used in foods subject to
this standard. All additives used shall be of food grade quality.
All food-grade salt, used in household and food processing should be fortified with
iodine as a safe and effective strategy for the prevention and control of iodine deficiency
disorders in populations.
Iodine contents at manufacturing stage shall not be lower than 30 ppm. Potassium
Iodate (KIO3) shall not be lower than 50 ppm on dry weight basis with one year of
manufacture. Iodine contents at distribution channel and at retail level 15 to 25 parts per
million on dry weight basis.
Iodization agent.
1. Potassium Iodate (KIO3), Calcium Iodate may be used for iodine fortification of salt.
Potassium Iodate and Calcium Iodate do not need stabilization agent
2. Potassium Iodide (KI) may be used for iodine fortification of salt but it needs
stabilization agent.
Step-1
Make Dry Mixture (KIO3)
(Anti-caking agents)
Calcium Carbonate
Potassium iodate (KIO3) Or
Tricalcium phosphate
Or
Magnesium carbonate
Ratio 1 : 9
Step-2
Make Premix (KIO3)
Ratio 1 : 10
Step-3
Salt Iodization
Premix Salt
KIO3+ Salt
Bulk Salt
(Ratio 1:2000)
Rotary Valve
to Adjust Ratio
Dry mixing of salt with KIO3 is possible only if the salt is dry and finely ground.
Otherwise the KIO3, having a finer particle size and being heavier than salt, will settle at
the bottom of the container. This method is therefore not recommended for the unrefined
coarse salt that is commonly used in developing countries.
Wet Mixing
In the wet method, potassium iodate is first dissolved in water to make a concentrated
solution. This solution can be either dripped or sprayed on the salt at a uniform rate.
Step.1 The Salt is fed into a hopper (capacity of about 300 kg) that discharges at a
uniform rate onto a belt conveyor, about 35-40 cm wide and 5.5 m long inclined at a slope
of about 20 degrees. The conveyor is equipped with a tensioning device. The rate of salt
flow onto the conveyor is controlled by a slide valve.
Step.2 Flexible rubber curtains on three sides shape the salt into a narrow band 10-12 cm
wide and 2 cm deep on the conveyor belt and prevent it from spilling over the edge.
Step.3 The KIO3 solution is stored in two 200 litre polyethylene stock tanks with
discharge valves at the bottom to permit the filling of two 25 litre feed bottles, mounted to
ensure a continuous circulation of solution from the main tank to the feed bottles.
Step.4 The solution continuously drips at the desired rate onto the salt crystals.
Step.5 The iodized salt falls into a discharge hopper for collection in bags. For continuous
operation the hopper should have a twin spout with a diversion valve.
Note- i : The capacity of 5 tons per hour is ideal for a drip feed system, which requires
only a low pressure head to maintain the required flow rate.
Note-ii : This method is used in some Asian countries, for example, Indonesia. The drip
feed system is simple and cheap and is often used for iodizing moist crude salt crystals
and even refined powder salt.
Note-iii : In a simplified system used in India, the drip system is introduced into the feed
point of a salt grinder. The drip feed system followed by grinding often yields consistent
iodate dispersion.
2. Spray Mixing
when the particle size of the salt is very fine (less than 2 mm), the spray-mix
method is better because it atomizes the iodate solution and sprays it as a mist, thus
mixing it uniformly with the salt. The spray-mix method is also preferable to the drip feed
system when the salt varies in particle size and moisture content, as frequently occurs
when the iodizing plant receives salt from a number of different sources.
Salt iodization plants is required where refining equipment is not available. Large
salt lumps are crushed to a coarse powder in impact crusher and roller mill and after
passing through vibrating screen, fed into a feed hopper fitted. A rotary valve is fitted in
the outlet of the hopper and regulates the flow onto an inclined conveyor belt. The shafts
are driven by a variable speed drive system and the rate of rotation is adjusted to give the
required discharge.
The sheet of salt discharging from the belt into the spray chamber receives a fine
atomized spray of potassium iodate solution from two nozzles, at a pressure of 1.4 kg/cm2.
The spray nozzles are designed to deliver a flattened spray that spreads over the entire
width of the salt stream. The concentration of solution and the spray rates are adjusted to
yield the required dosage of iodate in the salt. The iodate solution is kept under pressure
in two stainless steel drums, each of about 80 liters capacity. The pressure in the drums is
maintained constant by an air compressor with a regulator. The salt with added
potassium iodate falls into a screw conveyor 20-25 cm wide and 2.5-3.0 m long. Travel
through the screw provides uniformity of mixing. The screw conveyor discharges into
twin outlets where bags are kept ready for filling. All the parts coming into direct contact
with salt are made of stainless steel, to minimize corrosion.
RIBBON BLENDER
The blenders are powered by suitable motors. The rotation is reduced through a
suitable gear box to give a speed of 20-30 rpm. The speeds and power requirements of
blenders of different capacities are given below:
125 kg 2.2 KW 3 HP
250 kg 3.7 KW 5 HP
500 kg 3.7 KW 5 HP
+ 1.5 kw (Elevator) +2 HP (Elevator)
The spray system atomizes the iodate solution and disperses it uniformly on the
salt crystals, thus ensuring much more uniform mixing when compared to the drip feed
system for all kinds of salt. The equipment requirements for the spray system and their
maintenance are a little more elaborate.
This method is simple to operate in the capacity range 0.5-3 tons/hour. It is already
being used in India, Peru, Vietnam.
Since the amount of KIO3 is so small, it will have to be supplied in pre-weighed packets
because accurate balances will virtually never be available in villages choosing this
approach.
The chemist should collect samples of iodized salt at regular intervals as it flows
out of the chutes. He should analyze them immediately for iodine content, and advises the
plant operator to take corrective measures, as needed, by adjusting the flow of salt/spray.
This analysis must be very prompt to permit effective control of levels.
Iodized salt should be collected into bags directly as it flows out of the chutes
instead of allowing it to fall onto the ground, because any moist crystals may pick up dust
and dirt.
All the bearings should be well greased so that the operational efficiency of the
plant is maintained. Jammed rollers and slow-moving belt conveyors will give uneven
iodization.
Folate, also known as vitamin B9 and folacin, is one of the B Vitamins manufactured folic
acid, which is converted into folate by the body, is used as a dietary supplement and
in food fortification as it is more stable during processing and storage. Folate is required
for the body to make DNA and RNA and metabolise amino acids necessary for cell
division. As humans cannot make folate, it is required in the diet, making it an
essential nutrient. It occurs naturally in many foods.
Folate (as a fortification ingredient, folic acid) functions in reducing blood homocysteine
levels, forming red blood cells, proper growth and division of cells and preventing neural
tube defects
Building Requirements
For a 5 tons/hr plant working 8 hours a day, the daily requirement of salt is 40 tons.
Assuming a raw salt stock of 15 days and a finished product stock of 15 days, the total
storage capacity should be 1200 tons. On this basis, the building area is estimated in this
table which estimates the required building area for 5 ton/hr, single shift plant
Office 16
Switch room 6
Laboratory 9
4.g .
2 Lab. Dish
Size 2 to 3 inch dia.
3 Numbers
1000 ml = 1 number
500 ml = 3 numbers
500 ml = 3 numbers
1000 ml = 1 number
500 ml = 2 numbers
200 ml = 2 numbers
Quantity = 6 numbers
50 ml = 1 number
30 ml = 1 numbers
20 ml = 1 numbers
10 ml = 1 numbers
5 ml = 1 numbers
100 ml = 1 number
Quantity = 1 number
150 ml = 1 number
100 ml = 1 number
50 ml = 1 number
25 ml = 1 number
Quantity = 1 number
Quantity = 3 Liter
Quantity = 6 Numbers
conical flask
with stopper = 1 Number
Sulphuric acid to solution of iodized salt which liberates iodine, which is titrated with
sodium thiosulphate. Starch is used as an external indicator. Potassium iodide solution is
added to keep the Iodine in the dissolved state.
Arrange Reagents:
1. Sodium thiosulphate (Na2S2O3)
2. 2 N Sulphuric acid (H2SO4)
3. Potassium iodide (KI, AR)
4. Soluble chemical starch
5. Double Distilled Water.
Preparation of Reagents:
Sodium thiosulphate (Na2S2O3)
Dissolve 1.24 g Na2S2O3 in 1 Liter boiled, double-distilled water. This volume is sufficient
for testing 200 salt samples. Store in a cool, dark place. Properly stored, the solution can
be kept for a few months.
Add 0.6 ml concentrated H2SO4 slowly To 90 ml double – distilled water. Add boiled,
double-distilled water to make 100 ml. This volume is sufficient for 100 salt samples. store
in a cool dark place. The solution may be kept indefinitely.
Dissolve sodium chloride (NaCl) reagent (AR) in 100 ml boiled, double-distilled water.
While stirring, add NaCl until no more dissolves. Heat the contents of the beaker till
excess salt dissolves. While cooling the NaCl crystals will form on the sides of the beaker.
When it is completely cooled, decant the supernatant in a clean bottle. This can be stored
for 3 to 4 weeks.
Step-7 Slowly
Step-10
Step-9
1. Go on with Titration with
Add 1% starch solution Sodium Thiosulphate (from
to the flask (1 to 5 ml) buret)
till solution turns 2. Stop Till solution becomes
deep purple colorless
Step-11 (End)
Note Buret Reading
and check value
corresponds in table
for iodine PPM
S.No. Procedure
1 Carefully weigh 10 g of the salt to be tested.
2 Pour the salt into a 50 ml measuring cylinder.
3 Slowly add boiled, double-distilled water
4 Shake to dissolve the salt completely
5 Add more water to make 50 ml
6 Pour the salt solution (50 ml) into a conical flask with stopper
7 Pipette out 1 ml of 2 N Sulphuric acid and add this to the salt solution
8 The solution turns yellow; Close the flask with the stopper and put it in
the dark for 10 minutes. A closed box, cupboard or drawer may be used.
9 Pipette out 5 ml of 10% potassium iodide and add this to the salt solution
10 The solution turns yellow; Close the flask with the stopper and put it in
the dark for 10 minutes. A closed box, cupboard or drawer may be used.
11 Pour sodium thiosulphate into a burette.
12 Adjust the level in the burette to ‘0’
13 After 10 minutes, take the flask out of the dark box
14 Shaking the flask, titrate the solution in the flask with sodium
thiosulphate from the burette
15 Stop titration as soon as the solution turns pale (becomes very light
yellow)
16 Add a few drops (1 to 5 ml) of 1% starch solution to the flask
17 The solution turns deep purple
18 Continue titration until the purple coloration disappears and the solution
becomes colourless
19 Note the burette reading
20 From the attached table, read the iodine content of the sample in parts
per million.
Daily reports of the findings are made and the supervisor is to be alerted if the
iodine content is less than the prescribed level. Your report will lead to action to
protect the consumer. Delay on your part will delay these actions and harm the
consumer.
Date of Testing
Sample Number
Batch number of the Salt.
Date of Iodization
Where the sample was taken from?
Date of sampling.
REAGENTS DATA:
Water distillation.
RESULT
Titration Burette Reading.
Corresponding ppm from table of iodine contents.
Sign:
Name ________________________________
(Name and Signature of Analyst)
d. Boiling chips - Carborundum #12 granules, Cat. No. 133-B, Hengar Co.
f. Drying oven - FREAS oven Model 625, Cat. No. 51221139, Precision
Scientific
FeNH4(SO4) 2•12 H2O - ACS Grade, Cat. No. 3070, RICCA Chemical
Company
b. Nitric Acid - reagent grade (HNO3) ACS Grade, Cat. No. 9601, J.T. Baker
2. Solutions
i. Weigh 0.2500 ± 0.0500 g of KCl that has been dried at 101 °±1 °C for 1
hour
± 10 min into a 250 mL Erlenmeyer flask and dissolve in 40 mL of
water.
iii. Titrate with the AgNO3 solution to a permanent light brown (salmon
colored) endpoint.
C SAMPLE PREPARATION
b. Add 25.0 mL of 0.1000 ± 0.0005 N AgNO3 solution, swirl flask until sample
and solution are in intimate contact, and then add 15 mL of conc. HNO3.
c. Add sufficient boiling chips and boil until meat digests. Add a small amount
of lactose to the reagent blank.
e. Add KMnO4 solution in small portions while boiling to turn solution dark
brown.. Continue boiling until color disappears. Continue adding small
portions of KMnO4 until solution retains dark color for several minutes
before clearing. Wash sides of flask with water..
NOTE: If solution retains color and will not become colorless, add a small
amount of lactose until color disappears.
NOTE: If titration with KSCN is less than 2 mL, repeat with a smaller
sample weight.
E CALCULATIONS
1. Procedure
ml AgNO3
where R = ratio of ----------------------
ml KSCN
2. Hazards
Nitric Acid - reagent Will cause severe burns to all body Prepare solutions in a
grade (HNO3) tissue. May be fatal if swallowed or fume hood. Store out of
inhaled. direct sunlight. Regulate
Will react with water or steam to contact with heat, water,
produce heat and toxic and corrosive and incompatible
fumes. materials.
Potassium Oxidizer, contact with reducing agents
Permanganate or combustibles may cause ignition or
(KMnO4) extremely violent combustion. Causes
burns to all tissue. Toxic metal fumes
may form when heated to
decomposition.