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1. Purpose : To define Test Method for determination of chemical and physical parameters

2. Scope : Covers Finished Product samples received from RBC Plant

3. Definitions/Abbreviation :------

4. Reference : IS 2124 : 2000 Sodium Bicarbonate

5. Description :

Sr. No. Activity

Refined Sodium Bicarbonate samples are analyzed as per NLSARBC/QAD/IP/01

Refined Sodium Bicarbonate (RBC)

Following parameters are analyzed

5.1 Total alkalinity (as NaHCO3)

5.2 Chlorides (as Cl)
5.3 Sulfate (as SO4)
5.4 Insoluble matter
5.5 Calcium and Magnesium (as Ca)
5.6 Iron (as Fe)
5.7 Moisture
5.8 pH (1 % aqueous solution)
5.9 Heavy metals Lead (as Pb), Copper (as Cu) and Arsenic (as As) by ICP – OES
5.10 Whiteness
5.11 Bulk Density
5.12 Sieve Analysis

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Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020
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5.1 Determination of Total Alkalinity (as NaHCO3)

5.1.1 Requirement:

1. Standard Hydrochloric Acid 1.0 N

2. Standard Hydrochloric Acid 0.1 N
3. Methyl Orange Indicator

5.1.2 Procedure

Weigh accurately 4.4 g of Finished Product and dissolve in 100 ml of freshly boiled and
cooled water contained in a conical flask. Add (2-3) drops of the Methyl Orange Indicator
and 50 ml of standard Hydrochloric Acid (1 N). Stir the contents thoroughly and further titrate
with standard Hydrochloric Acid (0.1 N) until the color of the indicator solution changes from
yellow to red. Calculate the total volume in terms of Hydrochloric Acid (1 N).

5.1.3 Calculation

Total alkalinity (as NaHCO3), percent by mass

NaHCO3 = 8.4·V·N/M
where
V – volume in ml of Standard Hydrochloric Acid (1N) required for
titration,
N – normality of Standard Hydrochloric Acid used, and
M – mass in g of Finished Product taken for the test.

5.2 Determination of Chlorides (as Cl) content

5.2.1 Requirement:

1. Conc. Nitric Acid

2. Silver Nitrate Soln.(0.1 N)
3. Nitrobenzene
4. Standard Ammonium Thiocyanate Soln.(0.1 N)
5. Ferric Ammonium Sulphate indicator

5.2.2 Procedure
Weigh accurately 20 gms. Material of Finished Product in a conical flask, Neutralize it with
Conc. HNO3 and then add 5 ml. of acid in excess. Boil the solution to expel any dissolved
Carbon dioxide gas, cool, Add 3 ml. of nitrobenzene and shake vigorously. Add 10 ml 0.1N
Silver Nitrate Solution to the flask and titrate it against Standard 0.1N Ammonium
Thiocynate Solution using Ferric Ammonium Sulphate Indicator until end point a permanent
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Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020
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faint reddish Brown color appears.

5.2.3 Calculation
3.547(10N1-VN2)
Chloride (as Cl), % = ---------------------------
M
where

N1 = Normality of standard Silver Nitrate Solution (0.1N)

N2 = Normality of Ammonium Thiocyanate Solution (0.1N)
V = Volume in ml. of standard Ammonium Thiocynate Soln consumed
M = Mass in gram of Finished Product taken for the test

5.3 Determination Sulfates (as SO4)

5.3.1 Requirement :
1. Gooch crucible
2. Weighing balance
3. Oven
4. 4N Hydrochloric Acid
5. Barium Chloride solu.

5.3.2 Procedure
Dissolve about 10gm of Finished Product in 100ml of water, add drop of methyl orange and
Carefully add hydrochloric acid or more till it is pink and then boil to drive off completely the
Carbon dioxide formed. cool and filter, if necessary, through a folded filter paper. Wash the
filter paper with DM water, collecting the filtrate and washing liquor in 500 ml beaker. Dilute
to 250 ml. Boil and add 10 to 12ml hot barium chloride solution drop by drop so that the
addition is in slight excess and continue boiling for 4 min to obtain a granular precipitate.
Allow to stand for 4 hr. And filter through a weighed sintered glass crucible or Gooch
crucible. Wash the precipitate till free from chloride and dry to constant mass at 105 to
110°C. Alternatively, filter through Whatman filter paper No. 42 and wash till it is free from
chloride. Ignite and determine as barium sulphate.

5.3.3 Calculation:
M1
Sulphate(as SO4),percent by mass = ----- x 41.15
M2
M1=mass in g of the barium sulphate,and
M2=mass in g of the dried sample taken for the test.

5.4 Determination matter insoluble in water

5.4.1 Requirement:
1.Weighing Balance
2.Hot plate
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Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020
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3.Gooch crucible
4.Oven
5.4.2 Procedure

Accurately weigh 10 gm. of Finished Product, dissolve it in 100 ml distilled water in a beaker
and heat to Boiling and cool. Filter the solution through a weighed Gooch or sintered glass
crucible (G No.4) and wash the residue till it is free from soluble salts. Collect the filtrate and
washing in a one liter graduated flask and dilute to mark. Preserve the solution so obtained
for subsequent tests. Dry the crucible along with the insoluble residue to constant mass.

5.4.3 Calculation:
M1 x 100
Matter insoluble in water, percent by mass = ------------
M2
M1=mass in g of the residue, and
M2=mass in g of Finished Product taken for the test.

5.5 Determination of Calcium & Magnesium

5.5.1 Requirement:
1. Std. EDTA solu. 0.02 N
2. Ammonia Buffer solu.
3. EBT Indicator

5.5.2 Procedure

Weigh exactly 10 gm of Finished Product, dissolve in DM water and add 10ml of ammonium
chloride-ammonium hydroxide buffer solution, 5 drops of Eriochrome Black T indicator
solution and titrate against standard EDTA solution till wine red colour of the solution
changes to pure blue end point. Note the EDTA solution (V1) used in the titration.

5.5.3 Calculation

Calcium and Magnesium (as Ca),

AxV
Percent by mass = --------- X 100
M

A= calcium equivalent in mg of 1ml of EDTA solution determined

V= volume in ml of standard EDTA solution
M=mass in g of Finished Product taken for the test

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Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020
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5.6 Determination of Iron as Fe

5.6.1 Requirement

1. Con.HCl
2. 10% KSCN
3. Standard Fe2O3 solution 1ml = 0.1mg
4. Nessler cylinder
5. Ammonium persulphate
6. 150 ml conical flask

5.6.2 Procedure
Take 10 gm of Finished Product in 150 ml conical flask add 20 ml Con. HCl and boil for few
minutes. Now transfer the solution in to 100 ml Nessler cylinder add 20 ml distilled water
and 1 gm of ammonium persulphate, mix well and add 15 ml 10 % KSCN solution and make
up to 100 ml mark by adding of distilled water, red coloration appears. For blank preparation
take another Nessler cylinder and follows the above procedure without adding sample add
standard iron solution of Fe2O3 1 ml = 0.1 mg to the blank Nessler cylinder till the red
coloration becomes same as in the sample. Note the consumed standard reading.

5.6.3 Calculation
Standard consumed ( ml )x 0.1 x 1000
Iron as Fe2O3 (ppm ) = -----------------------------------------------------
Sample taken for test

Iron as Fe (ppm) = Iron as Fe2O3 (ppm ) X 0.7

5.7 Determination of Moisture content

5.7.1 Requirement

1. Moisture Balance
2. Moisture dish

5.7.2 Procedure
Switch on the meter and set the temp. 55-600C, place the sample pan on the handler and
press “TARE” when stability indicator “0.000” is displayed. Now open the lid and place
approximately 5 gm sample on sample dish, close the lid and when stability indicator “0.000”
is displayed, press “START/STOP” key. The display will switch to percentage mode. When
the measuring operation has been completed, the heating indicator will disappear. Display
shows reading of moisture content in the sample.

Prepared By Checked By Approved By Issue no. : 01

Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020
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5.8 Determination of pH in 1 % solution

5.8.1 Requirement

1. Weighing Balance
2. pH Meter

5.8.2 Method of test

Weight 1 gm. of sample and dissolve in 100 ml of dm water in graduated flask. Check pH of
solution by pH meter.

5.9 Determination of Element by ICP – OES (As, Pb, Cu )

5.9.1 Requirement:

 Inductively Coupled Plasma Optical Emission Spectrometer (ICP – OES)

 Multi Element Standard solution (Arsenic, Lead, Cooper) 100ppm or 1000 ppm
 Nitric Acid, Suprapure grade
 Yttrium Standard Solution 1000 ppm
 Micropipette, 1 – 100 l & 1 – 5 ml
 Centrifuge tube PP / HDPE graduated with cap, 50 ml
 DI Milli Q water

5.9.2 Procedure

Open both the gas Argon and nitrogen and assure 150 PSI pressure in outlet of cylinder.

Open the knob of both gas from gas purification system and assure pressure 80 – 120 PSI
in outlet pressure gauge.

Check the air compressor for condensate water by opening the release knob in bottom of
tank and drain if water present. Close the knob tightly.

Open the valve of exhaust hood Switch ON the main powder from junction box followed by
all related switches.
Switch On the powder supply of ICP followed by chiller, maintain at 17± 2 °C and computer
system.

After starting of computer wait for some time. Select and Click Win Lab32, system show
status of plasma & spectrometer; wait till system shows √ mark.

Prepared By Checked By Approved By Issue no. : 01

Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020
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Click Plasma Icon, ON plasma by clicking ON switch and wait till plasma ignites.

Set nebulizer system and assure proper drainage of water. Dip the Nebulizer tube in fresh
water.

Click Flush and flushing for 2 – 4 minutes with water, followed by 10 % & 2 % nitric acid and
finally with water.

Stop flushing by clicking Flush and close Plasma icon.

Open Works space by clicking Wrk Spe. Icon.

Select Nirma icp and double click, Click Method icon and select RBC Method and click Ok.

Click Sample Information and select RBC Sample Information and click Open.

Feed desired sample information in sample progress table by clicking Sample details.

Change sample ID followed by initial weight and Dilute volume ml and Ok.

Click Analysis icon followed by Enable / Disable element, disable all element and then √
mark only Ca and close.

Analyze water blank by clicking Analyze blank icon and wait till completion of analysis and
record Ca count. Repeat again and again till Ca cps comes below one lac, if necessary
change water.

After coming Ca, cps below one lac again click Analysis icon followed by Enable / Disable
element, disable all element and then Enable all element and Ok.

Again click Analysis icon followed clear calibration blank, clear reagent blank, clear result
display, clear spectra display and new calibration.

Click Open and select RBC file and change date & description and click Ok.

Start analyze blank by clicking Analyze blank and wait till completion of run.

After completion of blank dip Nebulizer tube into 25 ppb mixed standard and start analyze
standard by clicking Analyze standard and wait till completion of run.

Run 50 ppb & 100 ppb mixed standard like 25 ppb standard.
Washed plasma by dipping Nebulizer tube into water and flush for few minutes by using
plasma table.

Dip Nebulizer tube in sample solution and run by clicking Analyze sample and wait till
Prepared By Checked By Approved By Issue no. : 01

Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020
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completion.

Click Plasma and flush with 10 % nitric acid followed 2 % nitric acid and water.
Switch Off plasma by clicking off key.

Click File followed by Utilities, Data Manager, select data, Report, click existing design,
Next, select disable / unable, select required data & Ok.

Click Next, Next, click Summary, Next, write report title, Left click date, Right click time,
Report name, Ok, Next, Next, Sample, Click Negative value zero, Next, Preview, Print or
Close and Exit through File.

Click File & Exit.

Switch off Computer system, Chiller; ICP main switch, air compressor, & all other
accessories switches followed Mains.

Close knob of both gases Argon and Nitrogen from gas purification system followed by
cylinder valve.

Drain water from air compressor as before.

Close valve of exhaust blower.

5.1.9.3 Result

i. Note down the results of Arsenic, Lead & Copper in ppm

5.10 Whiteness

5.10.1 Procedure
Switch on, ‘WARMING UP’ is displayed meter and “insert the whiteness standard plate into
the drawer of the main unit and close the drawer. Meter will automatically give standard
value i.e 85.2- Auto calibration procedure”. Remove the standard plate.

Fill the sample platter with sample and use the spoon with spatula to pack down the sample
Open the drawer and place the sample platter inside and close the drawer.
Press the MODE key to switch from standard plate check mode to measurement mode.
Note result and remove the sample platter.
5.11 Determination of Bulk Density

5.11.1 Requirement
Trip drop density apparatus
5.11.2 Procedure
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Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020
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Use trip drop density apparatus. Fill the metallic funnel with Sodium Bicarbonate which is
closed from the bottom with a sliding plate. Put cleaned 500 ml metallic beaker at its
bottom. Pull the sliding plate. The material will fall in the beaker. Level the beaker with
metallic plate. Weigh the material.

5.11.3 Calculation
Bulk Density g/l = 2 x Weight. Of Material

Sieve analysis
5.12 Requirement:
5.12.1
1. Weighing Balance
2. Electronic Sieve Shaker

5.12.2 Procedure
Weight accurately 100 gm of salt sample. Place it in sieve (-0.150 mm) with pan and cover
it. Set the power at 20 and time for 10 min. Tighten the knob and push start button. After 10
min, remove the sieve and weight the fraction collected in pan.

5.12.3 Calculation
W1 x 100
Sieve fraction (-0.150 mm) % by mass = ----------------
W2
W1= Weight of fraction collected in pan
W2= Weight of Sample taken
6. Quality Records:
Record No. Title Location Retention
Period
Daily Analysis Log Book- Refined Sodium
NLSARBC/QAD/LOG/01 QAD 3 years
Bicarbonate Plant
NLSARBC/QAD/FOR/01 Analysis report of Sodium Bicarbonate – Food Grade QAD 3 years
NLSARBC/QAD/FOR/02 Analysis report of Sodium Bicarbonate – Tech. Grade QAD 3 years
NLSARBC/QAD/FOR/03 Analysis report of Sodium Bicarbonate – Feed Grade QAD 3 years
NLSARBC/QAD/REG/03 Bagging Register of Refined Sodium Bicarbonate QAD 3 years
NLSARBC/QAD/REC/01 Analysis Record of Refined Sodium Bicarbonate QAD 3 years

Prepared By Checked By Approved By Issue no. : 01

Signature Issue Date : 01.10.2017

Designation Sr. Chemist Officer HOD Rev. no. : 01

Date 01.10.2020 01.10.2020 01.10.2020 Rev. Date : 01.10.2020