74 API SPECIFICATION 13A/ISO 13500
18.5.2 Calculation Fluid apparent viscosity
Calculate the test fluid viscosity, VA, expressed in centipoise from Equation (47):
R 600
VA (47)
2
where R600 is the viscometer dial reading at 600 r/min.
Record the calculated value.
19 Drilling-grade xanthan gum
19.1 Principle
19.1.1 Xanthan gum is a water-soluble polysaccharide, commercially produced by a distinct fermentation
process of Xanthomonas campestris, and shall not contain any other polysaccharide, such as starch, guar gum
or other naturally occurring polymers or their derivatives. The product may contain up to 3 % of a material
added specifically to enhance dispersibility or solubility of the product. Xanthan gum is an off-white, free-flowing
granular powder.
19.1.2. Xanthan gum is used in a wide variety of water-based drilling, workover or completion fluids as a
rheology modifier to develop low-shear-rate viscosity and enhance suspension properties.
19.1.3 This procedure is a simple and reproducible method for assessing the performance properties of
xanthan gum used in drilling operations. Other specifications may be established for pay-zone applications,
including stimulation, workover or completion operations.
19.1.4 Xanthan gum shall be free of any foreign polymer including cellulosics, starch or guar gum. Qualitative
tests should be performed to detect the presence of guar or starch, which are known to have synergistic effects
on the viscosity of xanthan gum solutions.
19.1.5 A solution of xanthan gum in synthetic seawater is used to determine the viscosity characteristics of
xanthan gum.
19.1.6 For optimum handling and mixing of the polymer in the field, it is recommended that the particle size of
xanthan gum powder be less than 0,4 mm (0,17 in; 425 µm). Xanthan gum shall conform to the specifications of
Table 18.
19.2 Qualitative starch determination in xanthan gum
19.2.1 Principle
[Link] The purpose of this test is to identify the presence of guar, starch and starch derivatives in xanthan
gum, supplied in powder or granular form. If starch is found, no further testing should be performed and the
sample shall be rejected.
[Link] An iodine/iodide solution is mixed with a solution of the xanthan gum being analysed. In the
presence of amylose (linear fraction of starch), a coloured complex is formed.
19.2.2 Reagents
[Link] Deionized (or distilled) water.
SPECIFICATION FOR DRILLING FLUIDS MATERIALS 75
Table 18 Xanthan gum physical requirements
Requirement Standard
Starch, guar, or their derivatives Absent
Moisture content Maximum 13 %
Screen analysis
Less than 425 µm (11/64 in) Minimum 95 %
Less than 75 µm Maximum 50 %
Viscosity a
Rotational viscometer, 300 r/min Minimum 11 cP 6)
(minimum 55 dial reading)
Rotational viscometer, 6 r/min Minimum 180 cP
(minimum 18 dial reading)
Rotational viscometer, 3 r/min Minimum 320 cP
(minimum 16 dial reading)
Brookfield LV, 1,5 r/min Minimum 1 950 cP
a For rotational viscometer, equipped with f0.2 torsion spring, R1/B1 configuration:
d) 300 r/min, cP equals the dial reading times 0,2;
e) 6 r/min, cP equals the dial reading times 10,0;
f) 3 r/min, cP equals the dial reading times 20,0.
[Link] Iodine solution, e.g. Merck 1.09.099.1000 (CAS No. 7553-56-2), 0,05 mol/l.
[Link] Potassium iodide, Merck 1.05043.0250 PA (CAS No. 7681-11-0).
[Link] Sodium hydroxide (NaOH) (CAS no. 1310-73-2), dilute, 0,1 % to 0,5 %.
19.2.3 Apparatus
[Link] Mixer (e.g. Multimixer® model 9B with 9B29X impellers, or equivalent), having each spindle fitted
with a single sine-wave impeller approximately 25 mm (1 in) in diameter, mounted flash side up.
[Link] Container, approximate dimensions: depth, 180 mm (7,1 in); d top, 97 mm (3-5/6 in); d bottom,
70 mm (2,75 in) (e.g. Hamilton® Beach mixer cup No. M110-D, or equivalent). An alternative container option is
a 600 ml glass jar.
[Link] Laboratory spoon.
[Link] Spatula.
[Link] Balance, accurate to 0,01 g.
[Link] Volumetric flask, 100 ml.
[Link] Pasteur pipette, plastic, or drop bottle.
[Link] Timer, mechanical or electric, accurate to 0,1 min.
[Link] pH-meter with pH-electrode (e.g. Thermo Russell type KDCW11).
[Link] Polymer-dosing device (Fann or OFI).
76 API SPECIFICATION 13A/ISO 13500
[Link] Test tube.
19.2.4 Procedure Preparation of the iodine/iodide solution for qualitative starch determination
[Link] To a 100 ml 0 1 ml volumetric flask, add 10 ml 0,1 ml of a 0,05 mol/l iodine solution.
[Link] Add 0,60 g 0,01 g of potassium iodide (KI) and dissolve by gently swirling the volumetric flask.
[Link] Fill to the 100 ml mark with deionized water and mix thoroughly. Record the day of preparation.
[Link] The prepared iodine/iodide solution shall be stored in a sealed container, in a dark, cool, dry place
and can be used for up to three months. After the date of expiration, the solution should be discarded and
prepared again.
19.2.5 Procedure Preparation of xanthan gum solution for qualitative starch determination
[Link] Prepare a 1 % solution of the xanthan gum under examination. Add 396 g 0,1 g of deionized
water to the container and add 4,0 g 0,1 g of xanthan gum at a uniform rate over a time interval of 60 s to
120 s. The xanthan gum polymer shall be added into the vortex away from the impeller shaft to minimize
dusting, preferably with a polymer-dosing device as mentioned in [Link].
[Link] After stirring about 5 min 0,1 min, remove the container from the mixer and scrape the sides of
the mixing container with the spatula to remove or dislodge any xanthan gum adhering to the container wall. Be
sure that all xanthan gum clinging to the spatula is incorporated into the solution.
[Link] Measure the pH. If the pH value is less than 10, raise the pH to 10 by adding, dropwise, dilute
NaOH solution.
[Link] Replace the container on the mixer and continue to stir. Total mixing time shall be 20 min 1 min.
[Link] Put 2 ml of the xanthan gum solution in a test tube and add, dropwise, in portions of 3 drops at a
time, up to 30 drops of the iodine/iodide solution.
[Link] 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.
[Link] After every 3 drop addition, gently swirl the test tube and compare the colour of the solution under
examination with the blank test. The colour comparison should be made against a white background.
19.2.6 Results
[Link] If the sample under examination gives a yellow colour comparable to one of the blank test, the
sample does not contain any starch or starch derivatives.
[Link] The development of a light green to dark blue colour, either in solution or as a precipitate, indicates
the presence of starch (amylose fraction).
[Link] The development of a light pink to reddish-brown colour is an indication of the presence of a highly
substituted starch, dextrine, or starches with a high amylopectin content.
[Link] The development of any other colour is a strong indication of the presence of starch or starch
derivatives.
[Link] Instant discolouration indicates the presence of a reducing agent, in this case, continue the
dropwise addition of the iodine/iodide solution. Compare the colour obtained with those of [Link] to [Link].
[Link] If any colour reaction is detected other than that mentioned under 19.2.5, the testing is abandoned.
