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IEC No.

:1312 00 5386
TIN No.: 08262711414

CHEMTOTAL LABS PVT. LTD.


17E/804, CHB, Jodhpur,
Rajasthan. INDIA-342001
E-mail: india@chemtotal.com
Ph:+91-9799716055,
An ISO 9001:2008 Company +91-291-2703946

METHODS OF TESTING
(For test methods not listed, follow the applicable compendium)
Particle Size (KTM004)
Shake 50 g product on an 40 ( 400 μm) mesh and 200 (74 μm) Tyler Standard Screens for 10 minutes using a
Cenco-Meinzer sieve shaker.
Loss on Drying (KTM003)
Spread 3-5 g product evenly on a tared weighing pan and weigh accurately. Dry in an oven at 105°C for 21⁄2
hours. Cool in a desiccator and reweigh.
Appearance
Qualitative evaluation.
Powder Color (KTM006)
Test method is available upon request.
Viscosity and Shear Ratio
- 1% gum in 1% KCl (KTM017)
Slowly add a dry blend of 2.5 g product and 2.5 g KCl to 245 mL deionized water in a 400-mL beaker while
stirring at 800 rpm using a low-pitched propeller-type stirrer. After stirring for 2 hours at 800 rpm, adjust the
temperature of the solution to 25°C (77°F), and measure the viscosity using the LV model of the Brookfield
viscometer at 60 rpm with a #3 LV spindle. Reduce the speed to 6 rpm and measure the viscosity - the
shear ratio is calculated by dividing the 6 rpm viscosity by the 60 rpm viscosity.

- 0.25% gum in Synthetic Tap Water (KTM091)


Slowly add 0.75 g product to 299 mL Synthetic Tap Water (deionized water containing 1000 ppm NaCl and
147 ppm CaCl2·2H2O) in a 400-mL beaker while stirring at 800 rpm using a low-pitched, propeller-type
stirrer. After stirring for 2 hours, adjust the temperature to 25°C (77°F), and allow to sit undisturbed for 30
minutes. Do not stir. Measure the viscosity using an LV model of the Brookfield viscometer with a #1 LV
spindle at 3 rpm after allowing the spindle to rotate for 3 minutes.
Solution pH (KTM005)
Slowly add 3 g product to 297 mL deionized water in a 400-mL beaker while stirring at 800 rpm using a low-
pitched, propeller-type stirrer. After stirring for 30 min, measure the pH of this solution using a pH meter.

E-mail : india@chemtotal.com • Website : www.chemtotal.com


IEC No.:1312 00 5386
TIN No.: 08262711414

CHEMTOTAL LABS PVT. LTD.


17E/804, CHB, Jodhpur,
Rajasthan. INDIA-342001
E-mail: india@chemtotal.com
Ph:+91-9799716055,
An ISO 9001:2008 Company +91-291-2703946

II. TESTING PROCEDURES


a. Required equipment and glassware:
1. Fann Multimixer 9B with 9B29X impeller blades or equivalent. No load
speed: 11.500 rpm +/- 300 rpm.
2. Mixing cup for Fann Multimixer
3. Electric scale, accuracy 0.01gms
4. Model 800 Viscometer, OFITE, 8 speeds c/w f0.2 torsion spring, R1B1
configuration.
5. Timer, electric, accurate to 0.1 min
6. 1000ml cylinder, 1000ml glass cup.
7. 100ml volumetric flask
8. Stirring glass rod

b. Required chemicals:
1. Guar gum sample.
2. Pure NaCl (Sodium Chloride) salt for analysis purpose, Merck
3. Potassium Iodine
4. Sodium borate
5. NaOH 0.1M solution
6. NaOH dilute 0.2%
7. HCl 0.1M solution
8. Iodine solution
9. Distilled water

c. Procedures:

E-mail : india@chemtotal.com • Website : www.chemtotal.com


IEC No.:1312 00 5386
TIN No.: 08262711414

CHEMTOTAL LABS PVT. LTD.


17E/804, CHB, Jodhpur,
Rajasthan. INDIA-342001
E-mail: india@chemtotal.com
Ph:+91-9799716055,
An ISO 9001:2008 Company +91-291-2703946

I.1. Preparation of the Xanthan gum solution and starch determination


* Preparation of the iodine/iodide solution
- Add 10 ml ± 0,1 ml of a 0,1N iodine solution to 100 ml ± 0,1 ml volumetric flask, then add
0,60g ± 0,01g of potassium iodine (KI).
- Fill to the 100 ml mark with deionized water and mix thoroughly, record the day of
preparation.
* Preparation of the Xanthan gum solution and starch determination
- Add 4 g ± 0,1 g of Xanthan gum to 396 g ± 0,1 g of deionized water
- After stirring 5 min ± 0,1 min, measure the pH, raise the pH to 10 by adding, drop-wise, the
dilute NaOH solution. Continue to stir. Total mixing time shall equal 20 min ± 1 min
- Put 2 ml of the prepared solution in a test tube and add, drop-wise, in portions of 3 drops at a
time, up to 30 drops of iodine/iodide solution.
- Three blank tests using only deionized water with 3 drops, 9 drops, and 30 drops,
respectively, of iodine/iodide solution should be prepared for comparison.
- After every 3 drop addition, swirl the test tube and compare the colour of the solution under
examination with the blank tests. The colour comparison should be made against a white
background.
- If the sample under examination gives a yellow colour,the sample does not contain any starch
or starch derivatives.

The development of any other colour is a strong indication of the presence of starch or starch
derivatives. Instant discoloration indicates the presence of a reducing agent; in this case,
continue the drop- wise addition of the iodine/iodide solution. Compare the color obtained with
one of the blank test.

I.2. Qualitative Guar determination in Xanthan gum

E-mail : india@chemtotal.com • Website : www.chemtotal.com


IEC No.:1312 00 5386
TIN No.: 08262711414

CHEMTOTAL LABS PVT. LTD.


17E/804, CHB, Jodhpur,
Rajasthan. INDIA-342001
E-mail: india@chemtotal.com
Ph:+91-9799716055,
An ISO 9001:2008 Company +91-291-2703946

1.2.1. Preparation of the fresh Xanthan gum


- Add 1.5g ± 0.01g of Xanthan gum into 350g ± 1g fresh water. Mixing in 15 min ±1 min.
- Place the mixing cup in chilled water for not longer than 30min to lower the fluid
temperature to 25oC ± 1°C ( 77oF ± 2°F)
1.2.2. Preparation of the Sodium borate solution
- Add 10g ± 0.1 g of sodium borate into 90g ± 1.g of warm water in the beaker then stir with a
spatula for approximately 1 min to dissolve the sodium borate.
1.2.3. Viscosity measurement of the Xanthan gum solution
- Using the viscometer, measure the 300 reading, 6 reading and 3 reading of 250ml the above
fresh Xanthan gum sample at temperature of 25°C ± 1°C ( 77°F ± 2°F). Record the result as
R300-P, R6-P and R3-P.
1.2.4. Viscosity measurement of the Xanthan gum solution treated with Sodium Borate solution
- Add 30ml ± 2.0ml of sodium borate solution into the 250ml of the above sample which have
just had its viscosity measured. Hand stir with the spatula for 20s to 30s. Allow mixture to
stand for 5 min.
- Using the viscometer, measure the 300 reading, 6 reading and 3 reading of 250ml the
prepared Xanthan gum solution treated with Sodium Borate solution at temperature of 25°C ±
1°C ( 77°F ± 2°F). Record the result as R300-M, R6-M and R3-M.
1.2.5 Result interpretation.
- Compare the readings for the polymer solution (R300-P , R6-P, R3-P) and the mixture of
polymer and sodium borate (R300-M R6-M R3-M).
- Any increase between mixture readings and polymer solution readings indicates the presence
of guar in Xanthan gum.

I.3. Fluid viscosity.

E-mail : india@chemtotal.com • Website : www.chemtotal.com


IEC No.:1312 00 5386
TIN No.: 08262711414

CHEMTOTAL LABS PVT. LTD.


17E/804, CHB, Jodhpur,
Rajasthan. INDIA-342001
E-mail: india@chemtotal.com
Ph:+91-9799716055,
An ISO 9001:2008 Company +91-291-2703946

1.3.1. Preparation of synthetic seawater


- Add 41.95g of sea salt (NaCl) into 983g of deionized water. Mix 15 mins, measure and adjust
pH to 8.2 - 8.5 with 0.1M NaOH or HCl.

1.3.2 Preparation of the Xanthan gum polymer solution


- Add 1.0g ±0.001g of polymer to 358g of synthetic seawater, mix for 30 min ±1min, eliminate
foam by adding 2-3 drops of defoamer to the fluid.
- Place mixing cup in chilled water for not longer than 30min to lower the fluid temperature to
25°C ± 1°C ( 77°F ± 2°F)
1.3.3. Measurement of the viscosity
- Measure the 600rpm, 300rpm, 200rpm, 100rpm, 6rpm and 3rpm at a solution test temperature
of 25°C ± 1°C ( 77°F ± 2°F) using the direct-indicating viscometer (Fann viscometer or
OFITE 8 speed viscometer with R1B1 configuration and F0.2 torsion spring)

E-mail : india@chemtotal.com • Website : www.chemtotal.com

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