NACE TM0173

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NACE Standard TM0173-2005Item No. 21205

Standard

Test Method

Methods for Determining Quality of Subsurface

Injection Water Using Membrane Filters

This NACE International standard represents a consensus of those individual members who have

reviewed this document, its scope, and provisions. Its acceptance does not in any respect

preclude anyone, whether he has adopted the standard or not, from manufacturing, marketing,

purchasing, or using products, processes, or procedures not in conformance with this standard.

Nothing contained in this NACE International standard is to be construed as granting any right, by

implication or otherwise, to manufacture, sell, or use in connection with any method, apparatus, or

product covered by Letters Patent, or as indemnifying or protecting anyone against liability forinfringement of Letters Patent. This standard represents minimum requirements and should in no

way be interpreted as a restriction on the use of better procedures or materials. Neither is this

standard intended to apply in all cases relating to the subject. Unpredictable circumstances may

negate the usefulness of this standard in specific instances. NACE International assumes no

responsibility for the interpretation or use of this standard by other parties and accepts

responsibility for only those official NACE International interpretations issued by NACE

International in accordance with its governing procedures and policies which preclude the

issuance of interpretations by individual volunteers.

Users of this NACE International standard are responsible for reviewing appropriate health, safety,

environmental, and regulatory documents and for determining their applicability in relation to this

standard prior to its use. This NACE International standard may not necessarily address all

potential health and safety problems or environmental hazards associated with the use of

materials, equipment, and/or operations detailed or referred to within this standard. Users of this

NACE International standard are also responsible for establishing appropriate health, safety, andenvironmental protection practices, in consultation with appropriate regulatory authorities if

necessary, to achieve compliance with any existing applicable regulatory requirements prior to the

use of this standard.

CAUTIONARY NOTICE: NACE International standards are subject to periodic review, and may be

revised or withdrawn at any time without prior notice. NACE International requires that action be

taken to reaffirm, revise, or withdraw this standard no later than five years from the date of initial

publication. The user is cautioned to obtain the latest edition. Purchasers of NACE International

standards may receive current information on all standards and other NACE International

publications by contacting the NACE Firstservice Department, 1440 South Creek Drive, Houston,

TX, 77084-4906 (telephone + I [281] 228-6200).

Reaffirmed 2005-04-07

Revised 1999-06-25

Revised August 1992Revised February 1984

Reaffirmed February 1983

Revised June 1976

Approved February 1973

NACE International

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Houston, Texas 77084-4906

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ISBN 1-57590-085-8

O 2005, NACE International

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TM0173-2005

Foreword

Corrosion engineers in the oil- and gas-producing industry are often charged with the responsibility

of evaluating and controlling the quality of injection waters. Unfortunately, much of the dataavailable are inadequate, misleading, or difficult to interpret. This standard was prepared to

provide standard test methods for use by these engineers in evaluating water quality for injection

waters.

This standard was originally prepared in 1973 by NACE Task Group T-IC-12, revised in 1976,

reaffirmed in 1983, and revised in 1984 and 1992 by T-IC-20, components of Unit Committee T-

I C on Detection of Corrosion in Oilfield Equipment. T- IC was combined with T- ID on Corrosion

Monitoring and Control of Corrosion Environments in Petroleum Production Operations. This

standard was revised by T-ID-47 in 1999 and reaffirmed in 2005 by Specific Technology Group

(STG) 31 on Oil and Gas Production-Corrosion and Scale Inhibition. This standard is issued by

NACE International under the auspices of STG 31.

In NACE standards, the terms shall, must, should, and may are used in accordance with the

definitions of these terms in the NACE Publications Style Manual, 4th ed., Paragraph 7.4.1.9. Shall

and must are used to state mandatory requirements. The term should is used to state something

good and is recommended but is not mandatory. The term may is used to state something

considered optional.

NACE International I






TM0173-2005

NACE InternationalStanda rd

Test Method

Methods for Determining Quality of Subsurface InjectionWater Using Membrane Filters

Contents

1. General ......................................................................................................................... 1

2. Definitions ..................................................................................................................... 1

3. Description of Test Methods ......................................................................................... 2

4. Test Apparatus .............................................................................................................. 3

5. Preparation for Testing ................................................................................................. 6

6 . Test Conditions ............................................................................................................. 7

7. Test Procedures ........................................................................................................... 7

11

12

...................................................................................................................... 12Appendix A ........................................................................................................................ 12

Appendix B ........................................................................................................................ 13

Appendix C ....................................................................................................................... 15

Figure 1: Example of a membrane filter holder for 47-mm (1.8-in.) membrane filter. ........ 3

Figure 2: Membrane filter test apparatus showing membrane filter holder from Figure 1

Figure 3: Two-stage test apparatus with pressure gauge and regulator for repressurizing

and testing sample from reservoir rather than water-handling system (Figure 2), used

mainly when sample point cannot be easily adapted to on-stream application ............ 6Figure 4: Example of a graphic representation of water quality. ........................................ 9Figure 5: Apparatus for various washings or extractions by vacuum filtration. ................. 10

Table 1 Example of Membrane Filter Test Data.............................................................. 11

. .

connected to water-handling system 4

..II NACE International






TM0173-2005

Section 1: General

1.1 This standard describes two test methods for

evaluating water quality for subsurface injection: Procedure

A-rate versus cumulative volume test (for water-qualitymonitoring) and Procedure B-suspended solids test (for

diagnosis or monitoring). These two test methods are

intended to provide standardized water quality in the

petroleum production industry. The test methods describe

the apparatus required, test conditions, test procedures,

reporting procedures, and supplementary tests.

Interpretation of the results is beyond the scope of this

standard. The bibliography supplies sources of

interpretation methods.

1.1.1 Before establishing a test program, the aim of

the test should be determined and appropriate criteria

for evaluation of the test results should be established.

For example, if the intent is to use membrane filtration

as a simple water control test, the control criterionmight be a given slope of the filtration curve. If

diagnostic information is required, more emphasis may

be placed on qualitative information, such as the shape

of the filtration curve, or spot tests on the filtered solids

as well as visual examination of the filter immediately

after the test.

1.1.2 Membrane filtration may also be used to monitor

pickup of suspended solids from the formation, in

which case quantitative determination of solids on thefilter may be the selected criterion. Each situation

should receive an appropriate review of the parameters

involved

1.2 The injection behavior of subsurface formations varies

widely, and results of water-quality tests apply only to the

system being tested. Application of the results obtained by

these tests, therefore, is strongly influenced by the

requirements of each subsurface injection project. This

standard should be used for routine monitoring of water

quality, diagnosing of problems, evaluating effects of

system changes and upsets, and monitoring effects of

chemical treatment. The manner in which the test results

are used depends on the requirements of the specific

injection system.

1.3 This standard is applicable only when precautions are

observed to ensure that the sample is representative of the

water in the system of interest. It is not the purpose of this

standard to imply that the results or their interpretation may

be arbitrarily applied to other water injection projects.

Section 2: Definitions

2.1 Suspended solids, as used in this standard, are

defined as the nonwater, nondissolved substances that

exist in the water. These may typically include, but are notlimited to, materials such as iron sulfides and oxides,

precipitated carbonates and sulfates, sands and silts, oils,

paraffins and asphaltenes, and materials of biological origin.

The suspended solids may also be considered as the

materials in the water that can cause plugging and loss of

injectivity in injection wells.

2.1 I Oil carryover or hydrocarbon-soluble suspended

solids are the portions that are soluble in a suitable

hydrocarbon solvent. This standard is not intended to

be an accurate quantitative test for oil or hydrocarbons.

Oil carryover in the water cannot always be measured

by this technique because oil can pass through the

membrane filter. This method can give only a

qualitative indication of the oil carryover. Othermeasurement methods should be used when

quantitative data are desired. These methods are

listed in the bibliography.

2.1.2 Primary suspended solids or in-line suspended

solids are those substances that exist in the water at

the time of sampling.

2.2 Membrane filters, as used in this standard, refer to

porous disks composed of pure and biologically inert

cellulose esters. Unless specified to the contrary, the

membrane filters have a mean pore size of 0.45 pm (10.02

pm), a diameter of 47 mm (1.8 in.), a thickness of 15 pm

(I10 pm), and an average total pore volume of

approximately 80% of the total filter volume.

2.2.1 Preweighed membrane filters are those that

have been weighed prior to the test.

2.2.2 Matched-weight membrane filters are those

obtained from the supplier in pairs with identical

weights (I0 .02 mg).

NACE International 1




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TM0173-2005

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Section 3: Description of Test Methods

3.1 Rate versus Cumulative Volume Test (Procedure A)

3.1.1 This test method consists of passing a fixedvolume of injection water through a membrane filter

under constant pressure and measuring the flow rate

and cumulative volume of water at intervals.

3.1.2 This test is designed primarily for monitoring

injection water quality. A plot of the flow rate versus

cumulative volume of water gives a general indication

of the quality of the injected water.

3.2 Suspended Solids Test (Procedure B)

3.2.1 This test method consists of collecting samples

of primary solids as they exist in a water system. The

suspended solids from several liters of water are

collected on a membrane filter in a manner that permitslarger, more representative samples than those

obtained from bottle samples.

3.2.2 This test method provides a simple procedure for

collecting samples that are useful in the diagnosis of

problems encountered in handling water for subsurface

injection. The quantity of in-line solids and the

composition of these solids can be determined.

3.3 The suspended solids test and the rate versus

cumulative volume test may be run concurrently.

3.4 A number of supplementary tests are available to

identify the plugging material.

3.4.1 Microscopic Examination (See Appendix A)

3.4.1 I This test consists of viewing the

membrane filter with oblique incident light or

transmitted light, and inspecting the membrane

filter under a microscope. It is useful for

determining the nature of the plugging material in

injection systems.

3.4.2 Microchemical Spot Test Methods (See

Appendix B)

3.4.2.1 Sulfates. This test is specific for sulfates

and consists of adding acids and lead nitrate to a

membrane filter. Sulfate shows up as white,grainy reaction spots.

3.4.2.2 Silica. This test consists of adding

benzidine to a membrane filter and exposing it to

ammonia to develop a blue color.

3.4.2.3 Iron. This test consists of solubilizing the

iron in a solids sample on a membrane filter and

developing a blue color.

3.4.2.4 Protein. This test consists of filtering 1 L

of water through a membrane filter and dye

staining. A red stain that remains is an indication

of the presence of protein.

3.4.2.5 Iron Sulfide. This test consists of

dissolving the solids sample on a membrane filter

in hydrochloric acid containing sodium arsenite. A

bright canary yellow precipitate is formed if the

sample contains iron sulfide.

3.4.3 Hydrocarbon-Soluble Suspended Solids Test

(See Appendix C)

3.4.3.1 This test method consists of washing the

solids retained on the membrane filter as

described in Paragraph 3.2.1 with increments of

suitable solvents such as toluene, xylene, and

1 I I-trichloroethane until the filtrate is colorless.

The membrane filter is then dried and weighed.

The hydrocarbon-soluble suspended solids

content is calculated from the mass loss during

solvent washing.

3.4.3.2 The solvents referred to in Paragraph

3.4.3.1 are considered hazardous. Toluene and

xylene are flammable and present a fire hazard.

All of the solvents are harmful in the following

ways: (1) vapors are harmful to breathe; (2)contact with skin may cause chemical burns; (3)

solvents may cause severe eye damage; and (4)

solvents may cause death if ingested. Therefore,

the solvents must be used in fume hoods or other

properly ventilated areas. Eye protection and

appropriate clothing must be worn.

3.4.4 Acid-Soluble and Acid-Insoluble Suspended

Solids Test (see Appendix C)

3.4.4.1 This test method consists of washing the

membrane filter from the hydrocarbon-soluble

suspended solids test in Paragraph 3.4.3.1 with

warm hydrochloric acid. The membrane filter is

then rinsed with distilled water until chloride ionsare no longer detectable. The membrane filter is

dried and weighed. The acid-soluble and acid-

insoluble suspended solids contents are

calculated from the mass loss during the acid

wash.

2 NACE International






TM0173-2005

Section 4: Test Apparatus

4.1 The test apparatus consists of the membrane filters, be run on line as in Figure 2, a sample reservoir may bemembrane filter holders (shown in Figure I),ample used. Except as noted, the same apparatus is used for

receiver, sample connections and fittings, and pressure- ProcedureA and ProcedureB.regulation devices. As an alternative, when the test cannot

FIGURE 1: Example of a membrane filter holder fo r 47-mm (1.8411.) membrane filter. Construction is of

corrosion-resistant materials capable of withstanding upstream pressure of 14 MPa (2,000 psig). The holder

is designed for quick connection to a water-handling system to prevent detrimental aeration effects, and is

also designed for rapid assembly or dismantling.


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TM0173-2005

, Asample Manifold

Nipple

adlevalve \\

Toggle Valve*embrane Filter Holder

4raduated Cylinder

FIGURE 2: Membrane filter test apparatus showing membrane filter holder from Figure 1connected to water-

handling system. The 6.4-mm nominal OD (%-in. NPT) block and needle valves near the top keep system

pressure within set limits. Above the membrane filter holder is a quick-opening oggle valve to allow

immediate full-stream flow vital to timing accuracy. Length of tubing between the source and the apparatus

should be minimized o prevent forming a “dead leg.”

4.1.1 The pressure ratings of the test equipment

discussed in Paragraphs 4.3, 4.4, and 4.5 must be

strongly considered from a safety standpoint. When a

water injection system operating, for example, at 7, 14,or 28 MPa (1,000, 2,000, or 4,000 psi) is to be

sampled, the test equipment must be designed to

handle these pressures safely. This can be

accomplished by (1) selection of test equipment that

has the required pressure rating or (2) placement of a

proper pressure-relief valve located immediately

downstream from the injection system’s sample valve.

An alternative method that has been used is that

shown in Figure 2.4 in Applied Water Technology.’

4.2 Membrane Filter

4.2.1 The membrane filter defined in Paragraph 2.2

should be used for the rate versus cumulative volumetest (Procedure A). The diameter of the membrane

filter is less critical when only the suspended solids test

(Procedure B) is to be conducted, but a fixed diameter

should be used for all comparative tests. The

membrane filter should have a smooth surface to

permit easy removal of filtered solids.

4.2.2 Matched-weight membrane filters may be used

to help distinguish true suspended solids from







TM0173-2005

dissolved solids remaining after evaporation of water

held up by the membrane filter. Washing with

deionized water shall be done to remove dissolved

salts, because some waters are supersaturated in

soluble salts such as anhydrous calcium sulfate

(Caso,). The matched-weight membrane filters may

give a more accurate representation of true suspended

solids in systems for which these factors must beconsidered. Matched-weight membrane filters

(Paragraph 2.2.2) should be placed in a membrane

filter holder, superimposing one of a pair on the other.

The filter cake should be deposited on the upper

membrane filter, and filtrate should pass through both,

leaving behind an equal amount of dissolved solids on

both after evaporation of water held up by the filters.

NOTE: Membrane Filter Quality. Reasonable care

should be taken to ensure that membrane filters are

stored in a reasonable atmosphere. Membrane filters

stored under unusual conditions or for long periods of

time (years) should be discarded.

4.3 Membrane Filter Holder

4.3.1 The membrane filter holder should be

constructed of corrosion-resistant materials. For

safety, it must be capable of withstanding the pressure

at the sampling point unless upstream pressure relief is

provided.

4.3.2 The design should permit rapid assembling and

dismantling. The membrane filter holder should be

capable of ready connection to the water system to

prevent the effects of aeration. It may be constructed

of clear material to permit observation of the

membrane filter sutface during the test. Gas is often

trapped in the space above the membrane filter during

hookup. Provision should be made to remove this gaspocket before flow through the membrane filter is

started. A bleeder valve located on the top of the

membrane filter holder is an example.

4.3.3 The membrane filter holder should be

constructed to prevent water from leaking around the

edges of the membrane filter, and the membrane filter

holder should be free of sharp edges that could

petforate the membrane filter.

4.3.4 Figure 1 presents an example of a membrane

filter holder that embodies the basic requirements. It isnot necessary to duplicate the illustrated device if the

specifications given in Paragraph 4.3 are met. If

membrane filter diameters other than 47 mm (1.8 in.)

are used for Procedure B, the membrane filter holder

must be modified accordingly.

4.4 Sample Receiver or Reservoir

4.4.1 A graduated cylinder may be used as a sample

receiver when the test apparatus is connected as in

Figure 2.

4.4.2 If a two-stage test apparatus as illustrated in

Figure 3 is used, the calibrated sample reservoir must

be constructed to withstand pressures above 140 kPa

(20 psig). The reservoir should have a capacity of 3 to4 L and be calibrated in 20-mL increments. It should

be constructed of clear material to permit observation

of the water level and measurements of the filtered

volume. Reservoir components should be made of

corrosion-resistant materials.

4.4.2.1 Quantitative analyses of solids retained on

a membrane filter when using a calibrated sample

reservoir as shown in Figure 3 may be of little

value in many cases because of solids that form in

the calibrated sample reservoir while the water

sample is collected. It is virtually impossible to

remove all of the oxygen that is present in the

calibrated sample reservoir when it is purged withnitrogen prior to sampling the water. Precipitation

of solids may occur during sampling due to

pressure drop or reaction with oxygen. Therefore,

calibrated sample reservoirs should not be used

for the suspended solids test.





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TM0173-2005

FIGURE 3: Tw o-stage test apparatus with pressure gauge and reg ulator for repressurizing and testingsam ple from reservoir rather than water-han dling system (FIG URE 2), used m ainly when sample point

cannot be easily adapted to on-stream application.

4.5 Sample Connections, Fittings, and Pressure

Regulation

4.5.1 Corrosion-resistant fittings, valves, and tubing

should be used to connect the test apparatus. The

tests should be run with the membrane filter holder

connected directly to the system, using suitablepressure regulators and valves to set the test pressure

(Figure 2). If the entire test apparatus can withstand

system pressure, no pressure relief is required. If,

however, the system pressure is greater than the

recommended operating pressure of any item of the

test apparatus, pressure relief shall be provided with a

pop valve, rupture disk, or other device. The valves

and regulator system shall be capable of providing a

constant pressure of 140 kPa (20 psig) or higher.

4.5.2 If a calibrated sample reservoir (Figure 3) is

used, a suitable two-stage pressure regulator shall be

used for repressurization with nitrogen.

Section 5: Preparation for Te sting

5.1 Weighing (Taring) of Membrane Filters for the 5.1.2 The tare weight of the membrane filter should be

Suspended Solids Test (Procedure B) determined to the nearest 0.1 mg (constant weight).

5.1.1 The membrane filter should be washed with 250 5.1.3 The tare weight should be recorded on the

mL of warm (31 to 34°C [88 to 93"F]), clean distilled container (petri dish, plastic case, etc.) for each

water to remove manufacturing solvents and individual membrane filter.

sutfactants.

high-quality water. The membrane filter should be 5.1.4 When high-quality water is tested, the

dried at 60°C (140°F) for two hours, cooled in a membrane filter should be prewashed with deionized

desiccator to room temperature to prevent weight gain, water prior to weighing to remove trace amounts of

and weighed prior to its use in Procedure B. When soluble material in the membrane filter.

matched-weight membrane filters are used, the

washing and drying are not necessary.

This is particularly critical when testing







TM0173-2005

Section 6: Test C onditions

6.1 Cleanliness

6.1.1 Prior to each test run, all parts of the testapparatus must be clean.

6.1.2 The test points must be thoroughly flushed to

ensure a representative sample.

6.2 Test Temperature

6.2.1 If the membrane filter holder is attached directly

to the system, the test temperature at the sample point

shall be measured and recorded.

6.2.2 For a repressurized test, the temperature of the

water in the calibrated sample reservoir shall be

measured and recorded.

6.3 Test Pressure

6.3.1 The test pressure for the rate versus cumulative

volume test shall be 140 kPa (20 psig) ?IO% at the

membrane filter.

6.3.2 Test pressure should be obtained by suitable

mechanical devices for on-stream sampling and by a

pressure regulator between the nitrogen source and

the calibrated sample reservoir for repressurized tests.

6.3.3 The test pressure for the suspended solids test

(Procedure B) is not very important. However, if

pressures are too low, it is difficult to flow water through

the membrane filter and some pressure assistance isrequired.

6.4 Test Sample Volume

6.4.1 For routine rate versus cumulative volume tests,

the test sample volume shall be 2.5 L. When water

quality permits rapid filtration, test samples up to 10 L

or more may be required for meaningful interpretation.

Test sample volumes of 3 or 4 L are considered

adequate to determine representative conditions in

most systems using the suspended solids test.

6.4.2 Some waters are of such poor quality that almost

complete plugging occurs before the recommended

test sample volume can be filtered. There is no

worthwhile information to be obtained from continuing

to measure effluent from the near-plugged membrane

filter. In such instances the rate versus cumulative

volume test should be terminated short of “test sample

volume.”

6.4.3 The suspended solids test should be conducted

on several membrane filters to provide an aggregate of

3 to 4 L of filtered solution. The results of the latter

tests should be averaged. When membrane filters

plug after 25 to 100 mL, it may be impractical to obtainan aggregate of 3 to 4 L of filtered solution. However,

the test should be conducted on several membrane

filters to provide a large aggregate of filtered solution.

6.5 Test Sample Points

6.5.1 Special care must be taken to ensure that a

representative sample of the water is obtained. Test

samples must be taken at points that do not contain

matter from stagnant areas, large amounts of

macrosolids such as debris and matter not

representative of injection water, and at points that are

disproportionately conducive to collecting oil or solids.

6.5.2 Although adequate and appropriate testsampling points are seldom found in existing systems,

planning for new systems should incorporate test sites.

6.5.3 In existing systems, test samples shall not be

taken at high points that tend to collect entrained oil

and drop suspended solids or at low spots that tend to

lose oil and gain solids when compared with the main

st ream.

Section 7: Test Procedures

7.1 Test Preparation. The following procedures shall be

used in preparing for the test.

7.1.1 Carefully insert the test membrane filter in the

membrane filter holder with tweezers to avoid

damaging the membrane filter and to avoid bypassing

water at an edge.

7.1.2 Moisten the test membrane filter with warm,

clean distilled water.

7.2

7.1.3 Purge the test sample point and connecting

tubing thoroughly to remove any sludge or deposits

that may have accumulated in the valve or other

fittings.

Repressurization

7.2.1 If it is not feasible to conduct an on-stream test,

collect a water sample in the calibrated sample

reservoir, after purging free of air, under an

atmosphere of nitrogen. In some cases the pressure





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TM0173-2005

differential between the line and calibrated sample

reservoir allows precipitation of solids that will

invalidate conclusions concerning the quality of the

water in the system if based on further data from a

continuation of this test. In most cases this

precipitation can be visibly detected by rapid black or

red coloration of the water. (Note: This procedure

should not be followed for the suspended solids test.)

7.3 Air Venting

7.3.1 Displace any air from the test membrane filter

holder with test sample water by using the vent valve or

by inverting the membrane filter holder momentarily.

7.4 Procedure A (Rate versus Cumulative Volume Test)

7.4.1 Adjust the pressure to provide for a constant 140

kPa (20 psig) ?IO% at the membrane throughout the

test. A higher constant pressure may be selected or a

series of tests at various constant pressures may be

used. However, the pressure limits of the test

apparatus should be known and shall be adhered to.

7.4.2 Initiate flow through the membrane filter and start

timing to coincide with passage of the first drop through

the membrane filter.

7.4.3 Record the time and volume in one of these two

ways: (1) record the time for each 100-mL increment;

or (2) record the volume at selected time increments.

Continue the test until a specified volume is obtained or

until 600 seconds have elapsed, whichever is first (see

Paragraph 6.4.).

7.4.4 Conduct two or more tests at each sample point.

7.4.5 Test Completion

7.4.5.1 Upon obtaining the required volume of

filtrate, isolate the test membrane filter holder from

the pressure source.

7.4.5.2 Disconnect and dismantle the test

membrane filter holder and carefully remove the

test membrane filter with tweezers. If it is to be

used in the suspended solids test, protect the filter

cake from contamination.

7.4.5.3 The test membrane filter should be kept

moist with a wet blotter pad if it is to be sent to a

distant laboratory for analysis. The moisture

keeps the test membrane filter from adhering tothe storage container.

7.4.6 Calculations

7.4.6.1 Plot the results from this test on

semilogarithmic graph paper as illustrated in

Figure 4.





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TM0173-2005

FIGURE 4: Exam ple of a graphic representation of water quality. Cum ulative volume in mL is plotted on theabscissa, and the flow rate in mLls is plotted on the ordinate.

7.4.6.2 Cumulative volumes and cumulative times

recorded during the test should be used to obtain

the change in time (At), the change in volume (Av),

and the average rate (Av/At) for each measured

increment. The data should be tabulated as inTable 1 and graphically represented as in Figure

4. The cumulative volume in mL should be plotted

along the abscissa, and the rate in milliliters per

second (mus) should be plotted on the ordinate.

7.5 Procedure B (Suspended Solids Test)

7.5.1 Timing is not required for this test.

7.5.2 Record the cumulative volume through the test

membrane filter.

7.5.3 Conduct two or more tests at each sample point.

7.5.4 Using tweezers, remove the test membrane filter

and filter cake from the container and prepare them for

testing. Tweezers for handling test membrane filters

shall have broad, flat ends to reduce possible damage

to the membrane filter; pointed ends are notacceptable.

7.5.5 Wash the membrane filter with deionized water

to remove water-soluble salts.

7.5.5.1 Wash the membrane filter by vacuum

filtration in an apparatus as shown in Figure 5.

7.5.5.2 Rinse the test membrane filter until the

filtrate is chloride-free as evidenced by no

precipitate when 5% (0.25 N) silver nitrate

(AgN03) is added to 1O mL of washings.





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FIGURE 5: Apparatus for various washings or extractions by vacuum filtration. The vacuum s ource m ay beeither a vacuum pump or a water aspirator.

7.5.6 Dry the test membrane filters in glass petri

dishes (covers slightly ajar) in an oven at 60°C (140°F)

for two hours. (Matched-weight pairs must be carefully

separated before drying.)

7.5.8 Determine the test membrane filter mass to the

nearest 0.1 mg. If a matched-weight pair is used,

weigh each membrane filter separately or place each

member of a pair on opposite sides of a pan balance.

7.5.7 Allow the test membrane filter to cool to room 7.5.9 Calculations

temperature in its petri dish with the cover slightly ajar.

(For critical tests on high-quality water, the membrane

filter should be cooled in a desiccator.)

7.5.9.1 Divide the mass of the test filter cake in

milligrams by the volume filtered in liters. The

results are expressed in milligrams per li ter (mg/L).





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TM0173-2005

Table l-Example of Mem brane Filter Test D ata

Sample: Alpha Membrane Filter: 47-mm

(1.8-in.) diameter, 0.45-

pm pore size

Test Pressure: 140 kPa (?IO%) Time for 2,500 mL: 3 min, 36 s

Date: February IO, 1992

Volume (v) Time (t) (s) Av At Rate (AdAt) Comments

(mL) (mL) (4 (mus)

200 15.1 1O0 7.6 13.2

300 23.0 1O0 7.9 12.7

400 31 O 1O0

500 39.1 1O0

600 47.3 1O0

700 55.6 1O0

800 64.0 1O0

900 72.5 1O0

1,000

1,100

1,200

1,300

1,400

1,500

1,600

1,700

1,800

1,900

81 O

89.6

98.4

107.2

116.1

124.9

134.0

143.0

152.1

161.2

1O0

1O0

1O0

1O0

1O0

1O0

1O0

1O0

1O0

1O0

2,000 170.0 1O0

2,100 179.5 1O0

2,200 188.7 1O0

2,300 197.9 1O0

2,400 207.1 1O0

2,500 21 6.3 1O0

8.0

8.1

8.2

8.3

8.4

8.5

8.5

8.6

8.8

8.8

8.9

8.8

9.1

9.0

9.1

9.1

9.1

9.1

9.2

9.2

9.2

9.2

12.5

12.3

12.2

12.0

11.9

11.8

11.8

11.6

11.4

11.4

11.2

11.4

11.0

11.1

11.0

11.0

11.0

10.9

10.9

10.9

10.9

10.9

Section 8: Reporting Test Data

8.1 A report should be written after each series of tests and

should contain the following details:

8.1.3 Descriptions of the test sampling points.

8.1.4 A brief discussion of the test methods used,

noting any variations from the standard procedures.

8.1.5 Tabulation and graphic representation of rate

versus cumulative volume test results (Table 1 and

Figure 4) as described in Paragraph 7.4.6.

8.1.1 A complete description of the water-handling

system tested, including sources, mixtures,

dispositions, and daily volumes.

8.1.2 A flow diagram with line sizes and types (steel,

plastic, etc.).







TM0173-2005

8.1.6 Tabulation of suspended solids test data for 8.1.9 Recommendations for improvements, based on

each sample point in mg/L, ppm, or lb/1,000 bbl. observed results, and recommendations for future test

methods and frequency.

8.1.7 A description of the filtered solids as determined

by one or more methods in Appendix C. 8.2 Test Interpretation and Application

8.1.8 A discussion of the test results and their 8.2.1 This standard presents test procedures that

implications, including comparisons with any prior test should give reproducible results for comparativeresu ts. evaluations. As discussed in Paragraph 1.1, the use of

the results is beyond the scope of this standard.

References

1. C.C. Patton, Applied Water Technology, 2nd ed. (Norman, OK: Campbell Petroleum Series, 1987).

Bibliography

American Conference of Government Industrial

“Threshold Limit Values of Airborneygienists.”)

Contaminants and Intended Changes.” 1970.

ASTM D 3921 (latest revision). “Standard Test Method for

Oil and Grease and Petroleum Hydrocarbons in

Water.” West Conshohocken. PA: ASTM.”’

Barkman, J.H., and D.H. Davidson. “Measuring Water

Quality and Predicting Well Impairment.” Journal of

Petroleum Technology 24, 4 (1972): pp. 865-873.

Dosher, T.M., and L. Webber. “The Use of the Membrane

Filter in Determining Quality of Water for Subsutface

Injection.” In Drilling and Production Practice.

Washington, DC: American Petroleum Institute (APi),‘3’

1957: pp. 169-179.

Eylander, J.G.R. “Suspended Solids Specifications for

Water Injection from Coreflood Tests.” SPE‘4’

Reservoir Engineering 11 (1988): pp. 1287-1294.

Appe ndix A-Microscopic Exam ination

Although microscopic examination is not an absolute

means of identification, it is a useful tool for determining the

nature of the plugging material in injection systems.

Examination by viewing the membrane filter with oblique

incident light or transmitted light may be used.

When large particulate material (>IO pm) is present, it can

be viewed best by oblique incident light. Very small

particulate matter is best viewed using transmitted l ight.

Apparatus:

The microscope used in this analysis typically has an

inclined binocular body, a mechanical stage (two axes), a

multiple nosepiece to accommodate two or more objective

lenses, a substage condenser, and wide-field eyepieces

(usually IOX). Total magnification ranging from 30 or 40X

to 400 or 500X is optimum for almost any identification

application using oblique incident visible light.

I. Microscopic Examination Using Oblique Incident Any of the larger incandescent lamps that provide a suitable

Visible Light light source for this application. These microscope lamps

should be the types that are mounted on an inclining stand

and have a focusing condensing lens. An adjustable iris

diaphragm and ground glass and daylight glass filters are

des rab e.

(’)American Conference of Government Industrial Hygienists (ACGIH), 1330 Kemper Meadow Drive, Cincinnati, OH 45240(’)ASTM International (ASTM), 100 Barr Harbor Dr., West Conshohocken, PA 19428-2959.

(3)AmericanPetroleum Institute (API), 1220 L St. NW, Washington, DC 20005.(4) Society of Petroleum Engineers (SPE), 222 Palisades Creek Drive, Richardson, TX 75083-3836.







TM0173-2005

Materials: Plastic petri dishes

Stainless steel forceps

50 x 80-mm (2.0 x 3.0-in.) glass slides

Petroleum elly or other suitable grease

ProcedUre:

1. Use the dried membrane filter from either the rate

versus cumulative volume test (Paragraph 3.1) or the

suspended solids test (Paragraph 3.2).

2. Prepare a clean 50 x 80-mm (2.0 x 3.0-in.) glass slide

by coating it lightly and evenly with a thin film of grease.

Place the membrane filter on the greased slide. The grease

causes the membrane filter to lie flat and entirely in one

focal plane.

3. Do not use a cover slide in this application because

any contamination on the cover slide may be mistaken for

material retained by the membrane filter. If the membrane

filter is to be preserved for further examination, place the top

of a plastic petri dish over the filter to protect it from

atmospheric contamination.

4. Adjust the incident light source to approximately 40

degrees from horizontal. Examine the membrane filter at

low magnification and then at suitable higher magnification.

Manipulate the microscope stage making two mutually

perpendicular traverses across diameters of the membrane

filters.

5. The oblique incident light will strike the contaminants

on the membrane filter from the side, making differentiation

between fibers, glass, and metals possible.

II. Microscopic Examination Using Visible TransmittedLight

Apparatus:

Microscope and light source are the same as those used in

the microscopic examination with oblique incident light,

except that a IOOX oil-immersion objective lens is useful for

examining and identifying very tiny particulate matter.

Materials:


50 x 80-mm (2.0 x 3.0-in.) glass slides

45 x 50-mm (1.7 x 1.9-in.)No. 1 cover slides

Immersion oil-index of refraction-I .51

ProcedUre:

1. Use the dried membrane filter from either the rate

versus cumulative volume test (Paragraph 3.1) or the

suspended solids test (Paragraph 3.2). If the membrane

filter is not available, a suitable membrane filter may be

prepared by passing 1 L of fresh sample through a

membrane filter using the apparatus shown in Figure 5.

This membrane filter should be rinsed and dried by the

procedure described in the suspended solids test

(Pa ag a ph 7.5.5).

2. With the forceps, gently float the membrane filter,

sample side up, on a film of immersion oil in the cover of a

plastic petri dish. Draw the membrane filter over the rim of

the cover to remove any excess immersion oil from the

bottom of the membrane filter. Roll the membrane filter

onto a glass slide.

3. Place a clean No. 1 cover slide over the sutface of the

membrane filter, being careful not to trap any air bubbles

under the slide.

4. Adjust the light path from the light source so it is

reflected by the flat substage mirror up through the

substage condenser, through the oil-wet membrane filter,

and into the objective lens. The immersion oil renders the

membrane filter transparent and allows the particles on the

sutface of the membrane filter to be observed.

5. Examine the membrane filter at low magnification and

then under high-powered oil-immersion lens. When using

the drop of immersion oil on the sutface of the slide cover,

carefully lower the oil-immersion objective, using the coarse

adjustment, until the top of objective ust makes contact with

the oil drop. Do this carefully so as not to damage the

objective lens by grinding it into the glass slide. Use the

fine adjustment to bring the sutface of the membrane filter

into final focus.

6. Manipulate the microscope stage making two mutually

perpendicular traverses across diameters of the membrane

filter.

7. The use of transmitted light with the high-powered oil-

immersion lens (total magnification-I ,000X) makes it

possible to identify tiny objects such as diatomaceous earth,

sand grains, slime masses, iron bacteria such as

Sphaerotilus and Gallionella, fresh-water diatoms, and rust

fragments.

Appendix B-Microchemical Spot Test Methods

The spot-testing technique lends itself to quick chemical may be applied. After the sample on the membrane filter

analysis of matter collected on an inert surface (in this case, has been solubilized and dried, the membrane filter is cut

a membrane filter). Spot testing requires that the ion to be into a number of wedge-shaped segments. These

identified be dissolved or partially dissolved before reagents segments are then individually tested for the various ions.





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TM0173-2005

The cutting blade may leave enough contamination at the

edge of the segment to give a positive test, but the

contamination will not extend into the center of the segment.

The spot tests given in this appendix are for sulfates, silica,

iron, protein, and iron sulfide. NOTE: Various strong

inorganic acids are used as reagents in these tests, e.g.,

nitric and hydrochloric acids. All of these acids are

hazardous and may be harmful in the following ways: (1)

vapors are harmful to breathe; (2) contact with skin may

cause severe chemical burns; (3) acids may cause severe

eye damage; and (4) acids may cause severe damage to

the digestive system if ingested. Eye protection and

appropriate protective clothing must be worn.

I. Sulfates

Materials:

Lead nitrate reagent, saturated aqueous solution

containing 1 mL of concentrated nitric acid per 25 mL of

solution

6N nitric acid

6N hydrochloric acid

ethylene propylene (FEP) coated or lacquered


47-mm (1.847.) microfiber glass

Prefilter pad

50 x 80 mm (2 x 3 in.) glass slides

47-mm (1.8-in.) plastic petri dish and cover, fluorinated

Black membrane filter (if available)

ProcedUre:

1.

filter using apparatus described in Figure 5.

Filter 1 L of fresh sample through a black membrane

2. Place a 47-mm (1.8-in.) microfiber glass prefilter in a

plastic petri dish and add 1.5 mL each of 6N hydrochloric

and nitric acids.

3.acid-wet prefilter, sample side up, and cover the petri dish.

Roll the membrane filter containing the sample onto the

4. Allow the petri dish to stand for 10 minutes. To aid the

dissolution of the sample, place the petri dish in a 60°C

(140°F) oven during this period.

5.mm (2 x 3 in.) glass slide. Allow the membrane filter to dry.

Remove the membrane filter and place it on a 50 x 80

6. Wet a microfiber glass prefilter with approximately 3mL of lead nitrate. Roll the sample membrane filter, sample

side up, onto the prefilter and let it stand for 10 minutes. Ablack membrane filter should be used for the collection of

the sample.

7. Mount the membrane filter on a glass slide and view it

under low-power (50X) microscopic examination. Use

incident light.

Resu ts:

Sulfate is indicated by white, grainy reaction spots. If it is

necessary to analyze the sample collected on a whitemembrane filter, view the membrane filter by transmitted-

light microscopy.

II. Silica

Materials:

Ben~idine,'~)% ethanol

Ammonium hydroxide, concentrated

7.0-mm (0.28-in.) iltedwire gauzelhot plate

ProcedUre:

1. Filter 1 L of sample using apparatus described in

Figure5.

2. Place the membrane filter on wire gauze and heat

gently over a hot plate.

3.fumes.

Add one drop of benzidine and develop over ammonia

Resu ts:

A blue color indicates he presence of silica.

III. Iron

Materials:

6N hydrochloric acid

6N nitric acid

Potassium errocyanide solution-saturated aqueous

47-mm (1.8-in.) microfiber glass prefilter47-mm (1.8-in.) plastic petri dishes with covers

ProcedUre:

1.

using apparatus illustrated n Figure5.

Filter 1 L of fresh sample through a membrane filter

2. Solubilize the iron in the solids on the membrane filter

using the technique described in the procedure or detecting

sulfates (see Appendix B, Microchemical Spot Test

Methods, I. Sulfates, Procedures 3 through 5). It is not

necessary o dry the membrane filter.

3. While the membrane filter is still slightly damp from the

solubilizing procedure, add one drop of the potassium

ferrocyanide solution.

. . . . . . . . . . . . . . . . . . . . . . . . . . .

(5)NOTE: Benzidine has been listed by the American Conference of Government Industrial Hygienists (ACGIH) as a cancer-causing agent.





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TM0173-2005

Resu ts:

A vivid blue color indicates the presence of iron. This is a

very sensitive test for iron; the results can be affected by the

presence of very large quantities of copper or molybdenum,

but this is seldom a problem.

IV. Protein

Because all bacteria are composed in part of protein, a spot

test for the presence of protein suggests the presence of

bacteria. If the test is positive, microbiological test

procedures not included in this standard may be used to

determine the nature of these organisms.

Materials:

Stain solution (percent by weight in distilled water)

composed of:

Ponceau-S dye 0.2%

Trichloroacetic acid 3.0%

Sulfosalicylic acid 3.0%Acetic acid 5%

47-mm (1.8-in.) filter absorbent paper

ProcedUre:

1.

in the apparatus shown in Figure 5.

Filter 1 L of water through a membrane filter mounted

2. Immerse the membrane filter in staining solution for two

minutes, agitate gently, remove, and blot between filter

absorbent paper.

3. Place the membrane filter in an acetic acid rinse and

agitate gently. Rinse the membrane filter in a second acetic

acid bath, remove, and blot dry.

Resu ts:

The bottom side of the membrane filter edge outside the

filtration area will rinse free of the red stain; proteinaceousmaterial will absorb the stain and remain a vivid red color.

V. Iron Sulfide

Material:

One 118-mL dropper bottle

15% hydrochloric acid containing 1.0% sodium arsenite

(NaAson) and 0.05% liquid detergent.

ProcedUre:

1.

being examined.

Place a drop of the acid solution on the membrane filter

Resu ts:

If a bright yellow precipitate of arsenic sulfide is formed, the

sample contained iron sulfide.

2. Because some iron will be dissolved by the acid, a

yellow-orange solution may result. This should not be

mistaken for the yellow precipitate formed by the sulfide.

Appendix C-Supplementary Suspended Solids Test Method s

The suspended solids test described in Paragraph 3.2 of

this standard may be supplemented with additional tests to

identify the plugging material. When the effects of air on

the sample are considered important in these

determinations, the collection, transfer, and filtration of

these samples should be accomplished under air-free

conditions. Examples of procedures that may be used to

determine the composition and characteristics of the

suspended solids are listed below. (Many laboratories use

other standard procedures that would be satisfactory for

these determinations.)

I. Hydrocarbon-Soluble Suspended Solids Test

Materials:

ProcedUre:

1. Place the previously weighed membrane filter from the

suspended solids test (Paragraph 7.5) in the apparatus

shown in Figure 5. If matched-weight pairs are used, place

the two membrane filters in the apparatus with the filter

cake topmost.

2. Wash the membrane filter with 5-mL increments of

toluene until the filtrate is colorless or practically colorless.

A water aspirator pump or portable vacuum pump with a

suitable cold trap should be used to pull the solvent through

the membrane filter. Adequate ventilation and safety

precautions shall be used due to the nature of the solvents

used.

Toluene (USP) may be used in lieu of chlorinated 3. Wash the membrane filter with 5-mL increments of

solvents, taking care to use adequate ventilation petroleum ether until the last traces of solvent are removed

and the filtrate is colorless. Use the same apparatus and

safety precautions observed in the previous solvent wash.

Petroleum ether (30 to 60°C [86 to 140"Fl)

4.

until a constant mass is obtained.

Air dry solvent-extracted membrane filters overnight or







TM0173-2005

5. Weigh the membrane filter to the nearest 0.1 mg. 6. Calculate suspended solids as shown in Equation (1):

Record hydrocarbon-free membrane filter mass.

mass after water wash (mg)-mass after solvent wash (mg)

volume of sample through filter (L)hydrocarbon-soluble suspended solids = (1)

NOTE: Oil carryover in the water cannot always be

measured by this technique because oil can pass through

the membrane filter. This method can give only a

qualitative indication of the oil carryover. Other

measurement methods should be used when quantitative

data are desired.

II. Acid-Soluble and Acid-Insoluble Suspended Solids

Test

Material:

15% hydrochloric acid

2. Wash membrane filter with several 10-mL portions of

hot (50 to 60°C [I 22 to 140"Fl) 15% HCI until filtrate is

clear.

3. Rinse membrane filter with distilled water until all traces

of HCI are removed. (Filtrate pH should be >5 as

determined by a suitable test paper.)

4.

2 hours.

Dry membrane filter in drying oven at 60°C (140°F) for

5.minutes in a desiccator.

Cool membrane at room temperature for at least 15

ProcedUre: 6. Weigh cooled membrane filter to the nearest 0.1 mg.

1. Place membrane filter from hydrocarbon-soluble 7. Calculate suspended solids as shown in Equations (2)

suspended solids test in apparatus shown in Figure 5. and (3):

mass after solvent wash (mg) -mass after acid wash (mg)

volume of sample through filteracid-soluble suspended solids (mglL) = (2)

mass after acid wash (mg)

volume of sample through filter (L)acid-insoluble suspended solids (mglL) = (3)

For matched-weight pairs, the initial mass is not neededbecause the lower membrane filter has been subjected to

all liquids and its mass should be the same as that of the

one supporting the filter cake (Paragraphs 2.2.2, 4.2.1, and7.5.8).





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NACE TM0173

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