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Please complete the missing data in the data section and type a sample calculation for each. Write a proper discussion and conclusion. all equations are provided in the power point slides.
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Petroleum 303 Drilling Fluids Lab
Spring 2019
Name:
Lab Partner(s) name(s):
Date performed:
Title:
Chemical Analysis.
Purpose:
The purpose of the lab was to determine pH which is the hydrogen ions concentration in
a solution. Also, determining clay’s capacity to absorb cations in a solution by conducting a
methylene blue dye test. Also, determining the solution’s reaction with acid. Lastly,
determining the amount of chloride content in the fluid by conducting a chloride test,
determining the calcium content in the solution, and determining the total hardness of the
solution.
Procedure:
Do the following tests:
1.Measure the mud pH using the color-matching strips.
2.Determine the methylene blue capacity for the mud.
3.Perform the alkalinity tests on the mud (Pm) and on filtrate #1 (Pf and Mf)
4.On filtrate #2, perform the following:
5.Chloride test
6.Total hardness test
7.Calcium test
Data Evaluation and Calculations:
1. Report mud pH, methylene blue capacity, titration concentration and volume for
chloride, total hardness and calcium.
2.Calculate the bentonite equivalent, hydroxyl, carbonate, bicarbonate and lime content
of the mud.
3.Calculate total hardness as calcium and magnesium.
1. Measure the mud pH using the color matching strip.
2. Determine the methylene blue capacity for the mud.
a. Measure 10 cc of DI water
b. Add 2 cc of drilling fluid
c. Add 15 cc of 3% hydrogen peroxide.
d. Add 0.5 cc of sulfuric acid.
e. Boil gently for 10 minutes (do not boil to dryness).
f. Dilute to about 50 cc.
g. Add methylene blue to the flash in increments of 0.5 cc, until dye appears as a
blue or turquoise ring surrounding the dyed solids
3. Perform the alkalinity test on the mud (Pm) and on filtrate #1 (Pf and Mf).
a. On the Mud (Pm).
i. Measure 1 cc of mud into the titration vessel.
ii. Dilute with 25-50 cc of DI water
iii. Add 4-5 drops of phenolphthalein indicator solution.
iv. Titrate with 0.02 N standard sulfuric acid solution, until the pink color
disappears.
b. On the filtrate (Pf).
i. Measure 1 cc of filtrate into the titration vessel.
ii. Add 2-3 drops of phenolphthalein indicator solution.
iii. If the indicator turns pink add a 0.02 N (N/50) standard sulfuric acid
solution, drop by drop until the pink color disappears.
c. On the filtrate (Mf).
i. To the last sample add 2 or 3 drops of methyl orange indicator solution.
ii. Add a 0.02 normal (N/50) standard sulfuric acid solution, drop by drop
until the color of the indicator changes from yellow to pink.
iii. The end point can also be taken when the pH of the sample drops to 4.3
as measured by pH meter.
4. On filtrate #2, perform the following:
a. Chloride test
i. Measure 1 or more cm3 of filtrate into the titration vessel.
ii. Add 2-3 drops of phenolphthalein indicator solution.
iii. If the indicator turns pink, add a 0.02 normal (N/50) standard sulfuric acid
solution, drop by drop until the pink color is discharged.
iv. Add 25-50 cm3 of deionized water.
v. Add 5-10 drops of potassium chromate.
vi. Titrate with Silver Nitrate solution (0.0282N or 0.282N AgNO3)
b. Total Hardness test
i.
ii.
iii.
iv.
Measure 1 or more cm3 of filtrate into a 150-cm3 beaker.
Add about 2 cm3 of hardness buffer and swirl to mix.
Add sufficient hardness indicator (2-6 drops) and mix. A wine-color a
will develop if calcium and/or magnesium are present.
While stirring, titrate with EDTA solution (Standard Versenate) until
EDTA produces no further red to blue color change.
c. Calcium test
i.
ii.
iii.
iv.
v.
Measure 1 or more cm3 of filtrate into a 150 cm3
beaker.
Dilute the sample to 5.0 cm3 with deionized water.
Add sufficient NaOH buffer to produce a pH of 12-13.
Add sufficient calcium indicator to produce a pink to
wine-red color if calcium is present. Too much
indicator will obscure the endpoint. ( The addition of
several drops of methyl orange along with the calcium
indicator may improve the visibility of the endpoint.)
While stirring, titrate with standard EDTA solution
(Standard Versenate) until EDTA produces no further
red to blue color change.
Data:
5. Measure the mud pH using the color matching strip.
pH= 11 – 12
6. Determine the methylene blue capacity for the mud.
Methylene Blue (cc) = 6
Bentonite equivalent (lb/bbl) =
7. Perform the alkalinity test on the mud (Pm) and on filtrate #1 (Pf and Mf).
a. On the Mud (Pm).
H2SO4 [0.02 N ], (cm3) = 0.95
b. On the filtrate (Pf).
H2SO4 [0.02 N ], (cm3) = 0.45
Free lime equivalent (lbm/bbl) =
c. On the filtrate (Mf).
H2SO4[0.02N], (cm3) = 0.3
last point (Pf))
(include the amount from the
4. On filtrate #2 perform the following tests:
a. Chloride test
H2SO4[0.02N], (cm3) = did not turn to pink
AgNO3[0.28N], (cm3) = 1.3
Chloride concentration (mg/L) =
b. Total Hardness test
EDTA Volume (cm3) = 0.9
Hardness (mg/L) =
c.
Calcium test
EDTA Volume (cm3) = 1.8
Calcium content (mg/L) =
Calculations:
Discussion:
Conclusion:
Lab Report Grading Guideline


















No Title on first page of report
Missing cover page
Missing purpose section
Missing procedure
Procedure not complete or well explained
Data section missing
Data section handwritten and not in tables
Missing sample calculations
Missing units in calculations and tables
Calculations done incorrectly
Graphs done incorrectly (missing axis labels, units, etc)
Missing discussion section
Missing sources of error
Missing conclusion
Weak conclusion or discussion
Missing questions at the end of the report
Questions answered incorrectly
Late labs
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Lab #5
pH determination – The term pH is used to
express the concentration of hydrogen ions
in an aqueous solution. pH is defined by:
pH = – log[H+] where [H+] is the hydrogen
ion concentration in moles per liter. At
room temperature, the ion product constant
of water, Kw , has a value of
1.0 x 10-14
mole/L. For pure water,
[H+] = [OH-] =
1.0 x 10-7, and the pH is equal to 7.
The pH of a fluid can be determined using
either a special ph paper or a pH meter.
The pH paper is impregnated with dyes that
exhibit different colors when exposed to
solutions of varying pH. The pH meter is an
instrument that determines the pH of an
aqueous solution by measuring the
electropotential generated between a
special glass electrode and a reference
electrode.
The methylene blue dye test is especially
designed to determine the capacity of a clay
to adsorb cations from solution. The method
is particularly applicable to drilling muds, but
it can be effectively applied to aqueous
dispersions of powdered clay, cores, and
drilled cuttings.
Like all cation exchange methods, the
methylene blue test measures the total
exchange capacity of the clay system, and is
dependent upon the type and content of clay
mineral present. Only the reactive portions of
the clay are involved and such materials as
finely ground limestone, sand, or barite do
not adsorb methylene blue.
Since the methylene blue test measures a
fundamental clay property with ease and
accuracy, it can be used as a novel analytical
tool in many industrial clay applications.
Where only a single clay type is involved, an
accurate estimate of the active clay content
can be made.
Methylene blue Capacity =
Methylene blue (ml)/Drilling fluid (ml)
Bentonite Equivalent:
=5 x Vmethylene blue/Vdrilling fluid
= lb/bbl

Alkalinity refers to the ability of a solution or
mixture to react with an acid. The
phenolphthalein alkalinity refers to the
amount of acid required to reduce the pH to
8.3, the phenolphthalein endpoint. The
phenolphthalein alkalinity of the mud and
mud filtrate is called the Pm and Pf ,
respectively. The Pf test includes the effect of
only dissolved bases and salts while the Pm
test includes the effect of both dissolved and
suspended bases and salts.
At a pH of 8.3, the conversion of hydroxides to water and
carbonates to bicarbonates is essentially complete.
Pm = V0.02N
H2SO4/Vsample
Pf = V0.02N
H2SO4/Vsample
The methyl orange alkalinity refers to the
amount of acid required to reduce the pH to
4.3, the methyl orange endpoint. The methyl
orange alkalinity of the mud and mud filtrate
is called the Mm and Mf , respectively. All
values are reported cubic centimeters (cc) of
0.02 N (normality = 0.02) sulfuric acid per
cubic centimeter (cc) of sample.
As the pH is further reduced to 4.3, the acid then
reacts with the bicarbonate ions to form carbon
dioxide and water.
Mf = V0.02N
H2SO4/Vsample
The Pf and Mf tests are designed to establish the
concentration of hydroxyl, bicarbonate, and
carbonate ions in the aqueous phase of the mud.
At a pH of 8.3, the conversion of hydroxides to
water and carbonates to bicarbonates is
essentially complete. The carbonates originally
present in solution do not enter the reactions.
As the pH is further reduced to 4.3, the acid then
reacts with the bicarbonate ions to form carbon
dioxide and water.
Unfortunately, in many mud filtrates, other ions
and organic acids are present that affect the Mf
test.
The Pf and Pm test results indicate the reserve
alkalinity of the suspended solids. As the [OH-]
in solution is reduced, the lime and limestone
suspended in the mud will go into solution and
tend to stabilize the pH. This reserve alkalinity
generally is expressed as an equivalent lime
concentration. Converting the Ca(OH)2
concentration from 0.02N to field units of
lbm/bbl yields 0.26 lbm/bbl.
Thus the free lime is given by:
.26(Pm-(fw x Pf)) , where fw is the volume fraction
of water in the mud.
Lime content = .26(Pm-fw Pf) = lb/bbl
Assume fw = 1.0
To determine the chloride content of a drilling
fluid filtrate sample, the sample is titrated
with a standard silver nitrate solution, using
potassium chromate as an indicator. The
silver nitrate precipitates the chloride ion
producing a red color silver chromate, which
is taken as the endpoint.

Report the chloride-ion concentration of the
filtrate in mg/L
ml of 0.0282 AgNO3 x (1000) = Mg/l Cl-

ml of 0.282 AgNO3 x (10,000) = Mg/l Cl-

Water containing large amounts of Ca2+ and Mg2+
ions is known as hard water. These
contaminants are often present in the water
available for use in the drilling fluid. In addition,
Ca2+ can enter the mud when anhydrite (CaSO4)
or gypsum (CaSO4 2H2O) formations are drilled.
Cement also contains calcium and can
contaminate the mud. The total Ca2+ and Mg2+
concentration is determined by titration with a
standard (0.02N) Versenate (EDTA) solution. The
Versenate, an organic compound capable of
forming a chelate with Ca++ and Mg++. Chelation
is a type of bonding of ions and molecules to
metal ions.
The hardness test is sometimes performed on
the mud as well as the filtrate. The mud
hardness indicates the amount of calcium
suspended in the mud as well as the calcium
in solution. This test usually is made on
gypsum-treated muds to indicate the amount
of excess CaSO4 present in suspension.
Total Hardness as Calcium =
(400 x VEDTA(ml))/Vsample(ml) = mg/L
Total Hardness as CaCO3(mg/L) =
Ca (mg/L) x 2.5
General Lab Report Format
Think of the lab report as a scientific essay. It will contain the following sections:
TITLE: The title should summarize, as specifically as possible, the subject of the lab.
PURPOSE: A single, concise statement of the major objective(s) of the lab that answers one of the following:
What question or questions is this lab exercise designed to answer? OR What is this lab exercise designed to show
or prove? OR What hypotheses is this lab exercise trying to prove or disprove? Note: To make a hypothesis, you
must be able to provide support for that hypothesis, based upon your knowledge or literature research. A
hypothesis should be an EDUCATED prediction!)
PROCEDURE:
You should include the information necessary to allow someone to repeat what you did, such as:
-What data was used? Include information about the data such as the data source (i.e. Internet, observations,
models)
-Include definitions of key terms and anything else necessary to understand exactly what was done.
DATA & RESULTS ( combine into one section)
DATA: This is a record of all measurements and other observations encountered during the lab exercise.
Record data carefully and immediately. Do not rely on your memory! The most carefully made observations are
not useful if you do not record them accurately. Always include the units of physical quantities. You and your lab
partner(s) should complete all the work and make all of the observations together. It is very difficult to write a good
lab report if you have not done some part of the experiment! Do not copy the results of other groups unless
instructed to do so: To do so will be considered plagiarism! If you and your lab partner(s) disagree about an
observation, record your own. Present the data in a way that makes it easy to discuss and to infer conclusions
(Tables or graphs are often helpful!) Do not describe the procedure or discuss the data in this section — just
present your data! Graphs will sometimes be required or helpful. These should be drawn on graph paper or with a
computer. The horizontal axis should contain the independent variable (the one that is known), and the vertical axis
should contain the dependent variable (the one that you are observing or measuring). Each axis must be labeled.
The graph must be titled. The intervals on each axis must be consistent.
RESULTS: Separate from your lab notes, this section should contain a summary of the final data, presented in a
form that is most useful for interpreting the results. A short paragraph should be sufficient, along with any relevant
charts and graphs labeled will. Remember to title and provide legends for all graphs and tables. The graphs and
tables should be comprehendible independently of their association with the text. Results are usually dominated by
calculations, tables and figures; however, you still need to state all significant results explicitly in verbal form, (i.e.
Using the formula for slope, the rate of change of the data is V = 1.8m/s). Graphics need to be clear, easily read, and
well labeled. Number and Title tables and graphs. An important strategy for making your results effective is to
draw the reader’s attention to them with a sentence or two, so the reader has a focus when reading the graph. In
most cases, providing a sample calculation of each type is sufficient in the lab report. Be sure to point out trends
and identify any special features. State your key result in sentence form.
DISCUSSION: This is the most important part of the lab, as it is where you interpret your observations and results.
For each conclusion you should discuss its significance and whether or not it seems reasonable. In addition, be sure
that you answer any questions that were asked in the laboratory instructions. You should infer conclusions from
your data. For each conclusion, you should provide evidence from your data. Be sure to include a sample
calculation of each type used. Give explanations for and implications of any relationships observed. (When
interpreting a graph, infer conclusions based upon the slope of the line or lines.
Support your ideas with specific, quantitative references to the results of your analyses. How do your observations
lead to the conclusions you reached? Were the relationships what you expected from the underlying physical
principles? If a conclusion does not seem reasonable, can you find any error in your procedure which could have
affected your results? For each conclusion you should discuss its significance. Address any interesting questions
you may have had as you were working through the lab exercises. In addition, be sure that you answer any
questions that were asked in the laboratory instructions. Can you make any generalizations? Why or why not?
CONCLUSION: Summarize your results, the main points of your discussion, and how they relate to your stated
purpose of the lab.
You are to restate all the conclusions that were made in the discussion section. No discussion or explanation or
speculation should occur in this section! (Do not use the words “because” or “since” or “therefore”.) It is a good
idea to include how the main points of your discussion are connected in order to demonstrate the overall significance
of your findings and the concepts you learned.
Please do not tell me how much you enjoyed this experiment or how much you learned from it. Just give me
your conclusions!

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