1.

CLAY CONTAMINATION - METHYLENE BLUE CAPACITY TEST

1. Equipment [Ref. 6.4 a]

a. Methylene blue solution: 1 cm3 = 0.01 miliequivelent

b. Sulfuric acid 5 N
c. Erlenmeyer flask: 250 cm3
d. Burette: 50 cm3
e. Graduated cylinder (TD) : 50 cm3
f. Stirring rod
g. Hot plate
h. Magnetic stirrer and stirring bar (coated)
i. Whatman No. 1 filter paper, or equivalent
j. Balance: sensitivity 0.05 g

2. Procedure [Ref. 6.4 a]

a. Accurately weigh 2.0g barite and add to the Erlenmeyer flask containing 50 cm3 Deionized
water.
b. Add 0.5 cm3 sulfuric acid.
c. Mix well and boil gently for 10 minutes. Do not allow to boil to dryness.
d. Cool to room temperature and bring volume to about 50 cm3 with water (deionized).
e. Add methylene blue solution to the flask with the burette in 0.2 cm 3 increments while stirring
on the magnetic stirrer. After each addition, mix the contents of the flask for 30 seconds and
remove one drop of the suspension with the stirring rod and place on the filter paper. The
initial end point of the titration is reached when dye appears as a faint blue ring or halo
surrounding the dyed solids as shown in fig 11.1 of Reference 6.4a.
NOTE: For the best accuracy it is recommended that increments no larger than 0.2 cm3 be
used.

f. When the initial endpoint is detected, stir the flask for an additional two minutes and place
another drop on the test paper. If the blue ring is again evident, the two minutes end point has
been reached. If the ring does not appear, continue as in Par. 6.2e until a drop taken after
stirring two minutes shows the blue tint or halo.
g. Continue stirring an additional 10 minutes and place another drop on the test paper. If the
blue ring is again evident, the 10 minutes endpoint has been reached. If the ring does not
appear, continue as in Par. 6.2d until a drop taken after stirring 30 seconds shows the blue
tint.
 3. Calculation [Ref. 6.4 a]

The methylene blue capacity of barite (MBT) is calculated as follows:

methylene blue solution , cm 3
Barite MBT, meq/100 g 
weight of barite sample, g

4. References

a. “Recommended Practice Standard Procedure for Laboratory Testing Drilling Fluids”, API
recommended practice 13 I, Section 11, Fifth edition, June 1, 1995.
2. CEMENT CONTAMINATION

5. Equipment [Ref. 7.3 a, b]

a. pH meter: milivolt range potentiometer calibrated to show pH units for measuring the
potential between a glass-membrane electrode and a standard “reference” electrode.
Specifications are as follows:

1. The pH rang: 0 – 14.

2. Electronics type: solid state (preferred).
3. Power source: batteries (preferred).
4. Operating temperature range: 32oF – 150oF (0oC – 66oC).
5. Readout: digital (preferred).
6. Resolution: 0.1 pH unit.
7. Accuracy: 0.1 pH unit.
8. Repeatability: 0.1 pH unit.
9. Adjustment:
(a) Temperature compensation of electrode system.
(b) Slope of electrode system (preferred).
(c) Calibration setting of readout. (An instrument with the
Preceding internal temperature compensation is Preferred).

b. Electrode system: A combination system of a glass electrode for sensing H + ions and a
standard-voltage reference electrode, constructed as a single electrode (preferred). The body
of this probe should be constructed of durable material. A flat-end probe is preferred for
better protection and easier cleaning of the electrode. A waterproof connection to the meter is
recommended. Specifications are as follows:
1. Glass pH electrode response range: 0-to-14-pH unit.
2. Electrodes: a glass electrode and a silver/silver chloride electrode in
combination, having a ceramic or a plastic single or double junction.
NOTE: Use a double junction electrode for measuring liquids containing sulfide or bromide
ions to avoid damaging the (silver) reference electrode system.
3. Electrolyte in reference electrode: KCl gel.
4. Glass composition suitable for low-sodium ion error.
5. Sodium ion error at pH=13 or at 0.1 mole Na+ ion, an error less than 0.1 pH
unit.
 c. Buffer solutions: three solutions to calibrate and set the slope of the pH meter prior to sample
measurement.

1. The pH = 4.0 potassium hydrogen phthalate at 0.05 molar in water. Gives 4.01 pH at 75oF
(24oC).
2. The pH = 7.0: potassium dihydrogen phosphate at 0.02066 molar in water. Gives 7.00 pH
at 75oF (24oC).
3. The pH = 10.0: sodium carbonate at 0.025 molar and sodium bicarbonate at 0.025 molar
in water. Gives 10.01 pH at 75oF (24oC).

d. Distilled or deionized water in spray bottle.

e. Soft tissues to blot electrodes.
f. Thermometer: glass, 32oF – 220oF (0oC – 150oC).

6. Procedure [Ref. 7.3 a, b]

a. Use the filtrate prepared in part 2.2b as the sample. Allow it to reach 75 5oF (24 3oC).
b. Allow the buffer solution to also reach the same temperature as the fluid to be tested.
c. Check calibration validity, if not valid, calibrate the pH meter according to operating manual.
d. Clean the electrodes by washing them with distilled water, and blot dry.
e. Place the probe into the pH 7.0 buffer.
f. Turn on the meter; wait 60 seconds for the reading to stabilize.
g. Measure the temperature of pH 7 buffer solution.
NOTE: Discard and do not reuse the sample of buffer solutions used in calibration. The
meter should be fully calibrated every day as in Items b through k, using two buffers.
Check with the pH buffer every three hours.
h. If the meter calibrates properly, rinse the electrode with distilled water, and blot it dry. Place
the electrode in the sample to be tested and stir gently. Allow 60 seconds to 90 seconds for
the reading to stabilize.
i. Record the sample pH to the nearest 0.1 pH unit and the temperature of the sample tested.
j. Carefully clean the electrode in preparation for the next usage. Store in a vial of pH 4 buffer.
NEVER let the probe tip become dry.
k. Turn the meter off and close the cover to protect the instrument. Avoid storing the instrument
at extreme temperatures [below 32oF (0oC) or above120oF (49oC)].

7. References

a. “Recommended Practice Standard Procedure for Field Testing Water-Based Drilling Fluids”,
API recommended practice 13B-1, Section 9, Second edition, September, 1997.
b. PH meter operating manual