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CHAPTER 10

PETROLEUM LABORATORY OPERATIONS

Section I. Safety During Laboratory Operations

GENERAL PRECAUTIONS

All petroleum products present fire hazardsfor personnel who handle them. However, petro-leum laboratory personnel, who work with chemi-cals in close quarters, are exposed to additionaldangers. The chemicals handled may be toxic,corrosive, explosive, flammable, irritant, or car-cinogenic. Safe and efficient laboratory operationsdepend on the observance of well-establishedsafety practices and a thorough knowledge oftesting procedures. The testing procedures usuallyinvolve using equipment and materials that arepotentially dangerous. Injury to personnel anddamage to equipment by fire, chemicals, danger-ous pressures and vacuums, or misuse of equip-ment can be avoided by alert and responsible labo-ratory technicians. Each laboratory should haveoperating procedures that include all safety con-siderations. Strict observance of establishedsafety, care, and handling procedures will allowlaboratory personnel to perform their duties in asafe and hazard-free environment. All laboratorypersonnel should be familiar with safety aware-ness and communication issues concerning sub-stances used or tested at the facility. Also, Mate-rial Safety Data Sheets for those substancesshould be on hand. Some of the more commonsafety precautions that should be observed duringlaboratory operations are as follows:

• Do not consume any food or beveragesin the laboratory or storage rooms.

• Check for leaks in the oxygen, gas orvacuum systems by listening for hissing sounds,checking unexplained drops in pressure and ap-plying soapy water to the joints and fittings.

• Always have someone else with you inthe laboratory when performing test procedures.

• Pay attention to the test in progress. If itis necessary to leave the laboratory or to leave atest in progress, request assistance from anothertechnician or notify the supervisor. Make sure nosafety hazard will result from your absence.

• Maintain a professional manner in thelaboratory. Any unnecessary diversions can resultin increased hazards and unsatisfactory test re-sults.

• Do not attempt to perform tests simulta-neously unless each test can be given the requiredattention.

• Whenever in doubt concerning any op-eration, consult qualified authority for advice.

• Do not attempt unauthorized shortcuts tosave time, as they generally are not in accordancewith safe laboratory procedures or valid test re-sults.

• Be prepared for any emergencies thatmay arise. Be familiar with the proper action totake in event of emergencies.

• Protective gear (gloves, goggles, and ap-proved lab coat) should be worn when workingwith chemicals or fuels in the laboratory.

• Wear hearing protection when workingaround loud machinery (air compressor, generator,and so on).

• When ending daily operations, make athorough and orderly check of laboratory, equip-ment, and facilities to ensure that no hazards maydevelop during the time the laboratory is unat-tended. Inspections should be performed whenthe laboratory is unoccupied for an extendedlength of time.

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PREVENTING FIRES

Fire probably represents the greatest singlehazard in the laboratory. Laboratory personnelmust be aware of the potential sources of fire andwork conscientiously when handling combustiblematerials or supplies and samples that may formflammable vapors. Chapter 2 of FM 10-67-1, dis-cuses the properties of petroleum and their inher-ent fire hazards, safety procedures, and fire fight-ing practices. This should be required reading foranyone associated with petroleum products. Spe-cific to the petroleum laboratory, the following fireprevention rules, at a minimum, should be observedto prevent personal injury and equipment damage.

DO:• Inspect the laboratory for adequate venti-

lation.• Ventilate the laboratory and storeroom to

prevent the accumulation of fumes and vapors.• Check seals, tags, pressure gages, and

hoses of fire fighting equipment periodically tomake sure they are properly serviced and readyfor use.

• Inspect any apparatus you will be workingwith to ensure that it is fixed firmly in place.

• Check burner tubing frequently to ensurethat it is not faulty.

• Check electrical wiring frequently. Lookfor loose or defective connections or frayed insu-lation.

• Keep volatile liquids and flammable prod-ucts away from direct (engine exhausts, openflames, and direct sunlight) and indirect (circuitbreakers, switches, and electric motors) sources ofheat.

• Make certain there is no open flame orexposed heating element nearby when pouringhighly volatile liquids.

• Use glass beads or porcelain fragments, toprevent boiling over or splattering of liquids whenheating.

• Use flammable liquids near a source of ig-nition ONLY if the test procedures require it.

• Move flammable debris away from haz-ardous areas as soon as possible.

• Set hot liquids aside to cool in coveredcontainers before discarding.

• Break burned matches, or dispose of themin an ash receiver before discarding them in a ref-use container.

• Discard organic products in authorizedcontainers.

• Keep oily rags in a metal, airtight, closedcontainer.

• Immediately clean the area of a spill withabsorbent material. Dispose of this absorbentmaterial according to the installation waste dis-posal plan.

• Perform ohm tests every two years on allstatic grounds in the laboratory. (Maximum resis-tance is 25 ohms).

• Inspect to see that the funnel and funnelbase of the filtration apparatus have electricalcontinuity and are grounded.

• Store chemicals that are hazardous, whennear one another, in separate areas. (Oxidizersmust be kept separate from flammable and corro-sives.)

DO NOT:

• Smoke in the laboratory or associated ar-eas where chemicals are handled or stored.

• Leave open flames or heating elementsunattended.

• Discard organic products (hot or cooled)in sinks or drains.

• Store oily rags in cabinets or drawers.

MODULAR, MOBILE ANDAIR MOBILE LABORATORIES

The following procedures should be observedwhen operating in the modular, mobile or airmobilelaboratories.

• Purge the laboratory prior to entering. Ifthe purge system is inoperative, open all the doorsand vents, and wait at least 30 minutes before en-tering the laboratory.

• Ground the laboratory and generator.

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• Remove all waste drums and sample cansfrom the area when setting up or taking down thenets from the laboratory and equipment. (The netsgenerate static electricity.)

• Do not store empty or full sample cans inthe laboratory. Store empty or full sample cans ina protective area, at least 50 feet away from labo-ratory and generators.

• Test and calibrate the gas alarm system,as required.

FIRE EXTINGUISHERS

Trained personnel may use solid waterstreams, water sprays, and water fogs to controlor extinguish fires in specific situations. One of themost immediate means of extinguishing a fire iswith the use of a fire extinguisher. The Army usesboth portable hand extinguishers and wheeledunits. Portable hand fire extinguishers are effec-tive only in a fire’s earliest stages. Portable handfire extinguishers, except pump-tank units, areavailable in different sizes and types. The pump-tank unit uses water or an antifreeze solution(usually calcium chloride with corrosion inhibitors).Wheeled fire extinguishers offer more flexibilitybecause they have longer hoses and greater ca-pacities. Procedures for extinguishing fires shouldbe posted in the laboratory. Personnel should bethoroughly drilled in the areas of fire preventionand proper, quick response to the sighting of a fire.They should also be familiar with the nature ofpetroleum fires and with the fire extinguishingequipment in the laboratory. Fire extinguishersand other fire fighting equipment should be withineasy reach but safe from fire. In order for theextinguisher to be an effective tool, the followinggeneral rules must be followed.

• Know the location of and types of fire ex-tinguishers on hand in the laboratory, and theclasses of fires they are intended for.

• Inspect the laboratory facility monthly toensure that all extinguishers are in their designatedplaces, are readily accessible, are not damaged,and the nozzles are not clogged

• When using the extinguisher, follow themanufacturer’s instructions exactly.

• Recharge extinguishers immediately afteruse.

• All fire extinguishers must be tested.• Examine all fire extinguishers, at least

once a year or more often, depending on localregulations.

• Ensure that pressure-type extinguishersare tested hydrostatically.

• Testing should be performed on all fireextinguishers IAW current directives.

TYPES OF FIRE EXTINGUISHERS

The following paragraphs describe the morecommon types of fire extinguishers and their prop-erties.

Soda-Acid Extinguisher. The soda-acid ex-tinguisher is the most common type of water-solution extinguisher that uses gas pressure as theexpellent. The chemicals in the extinguisher aresodium bicarbonate (baking soda) and sulfuricacid. The sodium bicarbonate is in water-solutionform in the extinguisher, and the acid is containedin a loosely stoppered glass bottle. When someoneinverts the extinguisher, a chemical reaction pro-duces carbon dioxide that builds up pressure andexpels the water. Use this extinguisher type forClass A fires only.

Antifreeze Extinguisher. The antifreeze ex-tinguisher contains a calcium chloride solutioncharge. The expellant is gas from carbon dioxidecartridges or from a chemical reaction. The op-erator charges the extinguisher by inverting it andbumping it on the floor or by squeezing a valvelever. Use this type of extinguisher for Class Afires.

Loaded-Stream Extinguisher. The loaded-stream extinguisher is charged with an alkali-metalsalt solution and other salts. Potassium salts arepart of the charge. The way the agent works on afire differs with the class of the fire. It puts outclass A fires immediately and helps keep themfrom starting again. The way it works on smallclass B fires is unclear. The agent produces no

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smothering vapor, but there seems to be a chemi-cal reaction that tends to hold down combustion.

Carbon Dioxide Extinguisher. The carbondioxide extinguisher comes in many sizes. Thecharge of liquid carbon dioxide under 800 to 900-psi pressure is released by a hand valve at the topof the unit. A tube runs from the top to the bottomof the unit. This tube allows the release of onlyliquid carbon dioxide until the extinguisher usesabout 80 percent of its charge. Gaseous carbondioxide then flows until the charge exhausts. Thecharge flows in a high-velocity stream, and a hornor flaring nozzle keeps it from being diluted. Whenthe operator releases the charge and it enters thehorn, the chilling effect turns about 30 percent ofthe charge into dry ice or snow. Cooling of thegas as it expands causes this. Carbon dioxide di-lutes air in class B fires. It works well on class Cfires because it is not a conductor.

Dry Chemical Extinguisher. The dry-chemical fire extinguisher is available in a widerange of sizes. The chief agent is sodium bicar-bonate powder with additives that produce waterrepellency and free flow. The expellant is carbondioxide, nitrogen, or compressed air. The extin-guisher puts out the fire by smothering it. It workswell on class B and C fires.

Purple K Extinguisher. The purple K extin-guisher is a dry chemical extinguisher using theextinguishing agent potassium bicarbonate(KHCO3), commonly called purple K. Carbondioxide gas discharges the purple K in a widestream from a low-velocity nozzle. This fire extin-guisher works by smothering and is designed foruse on class B and C fires. Purple K is highly cor-rosive. Purple K extinguishers usually have a 20-pound capacity.

METHODS OF EXTINGUISHINGPETROLEUM FIRES

The following methods may be used to extin-guish petroleum fires, depending on the class ofthe fire. Table 10-1 illustrates the National FireProtection Association's four classes of fire, theirsource and extinguishing agent(s).

• Water and Water Fog. Water should beused as an absolute last resort for extinguishingpetroleum fires. Keep in mind that water is heav-ier than petroleum, and could cause the fuel tofloat thus spreading the fire. It is more effectiveas a cooling agent.

Table 10-1. Classes of Fire

Class of Fire Source of Fire Extinguishing AgentA Combustibles, such as: wood, paper, grass,

brush, rubbish.Water

B Liquid, such as: gasoline, and other fuels, sol-vents, lubricants, paints, oils, and similar sub-stances that do not leave embers.

Air-diluting agent, such as carbon di-oxide; or a smothering agent, such asfoam or a fire blanket.

C Electrical equipment, such as motors,switches, and transformers.

Air-diluting agent, such as carbon di-oxide or a smothering agent, such asfoam or a fire blanket. DO NOT usean agent that is a conductor of electric-ity.

D Combustible materials and other chemicals, Use a smothering agent, such as foam

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such as: sodium, potassium, titanium, andphosphorous. DO NOT allow water to comein contact with these substances, if ignited.

or a fire blanket.

• Blankets. Blankets are mainly used to putout a fire on a person's clothing. Wet blankets cansometimes be used effectively to help smother afire at a vapor leak or a vent.

• Carbon Dioxide. As opposed to water,carbon dioxide can be used on most petroleumfires.

• Sand. Sand can be used to cover or ab-sorb liquids for fire prevention. Sand is most use-ful in coping with fires caused by small quantitiesof flammable liquids and greases on the floor.

WARNING: Do not use water for extinguishingoil fires because it will spread the fire. Water isalso a conductor of electricity and should not beused on electrical fires.

HANDLING CHEMICALS

Many of the chemicals in the laboratory aredangerous. Any action associated with thesechemicals should be done safely. Broken or dam-aged containers must be handled with caution toprevent exposure of personnel to the hazards thatmay be involved with a particular chemical. Thefollowing safety precautions need to be observedby all personnel handling chemicals.

Personal Safety. To prevent personal injury inthe laboratory, the following safety measuresshould be employed.

• Wear rubber gloves when you handle ac-ids or bases.

• Wear goggles when it is necessary tobreak up chemicals, or when you handle quantitiesof corrosive liquids.

• Exercise caution when handling a 30 per-cent or stronger solution of hydrogen peroxide, toprevent contamination. Wash the area thoroughlywith water if skin becomes contaminated.

• Do not handle mercury with your barehands.

• Do not taste laboratory chemicals.

• Smell a chemical only when it is necessaryand then, only by wafting a small amount of vaporwith the hand, toward the nose.

• If any acid contaminates your skin, rinsethe contaminated area thoroughly with water. Theaffects of strong acidic solution may be lessenedby applying sodium bicarbonate (baking soda) afterrinsing the area with water. Consult a physicianimmediately.

Storing Chemicals. To prevent personal injurywhen storing chemicals in the laboratory, the fol-lowing measures should be employed.

• Make sure that every container and bottleis properly labeled.

• Store heavy and large containers ofchemicals on or as near to the floor as possible.

• Do not fill a container with material otherthan that indicated on the label.

• Store a standard solution of an acid or abase to avoid contamination by atmospheric CO2

(see Figure 10-1, page 10-6).• Do not store oxidizing agents with reduc-

ing agents.• Do not store acids and bases together;

they will react with each other.• Do not place bottles containing acids or

alkalis on high shelves or on top of equipment.Store them on low shelves so they can be easilyreached.

• Store caustic soda solution and sulfuricacid in strong glass containers, never in galvanizediron drums.

• Keep all sample containers capped orplugged at all times, except when pouring out testportions. Always replace the same cap or stopperin the container from which it was removed.

• Hold the stopper of a reagent bottle be-tween two fingers of the pouring hand whenpouring from a bottle. Never lay the stopper on asurface that might be touched by personnel or theirgarments.

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• Keep reagent bottles stoppered tightly, anddry reagent bottles before replacing them on theshelf.

• Wipe up any acid that spills or splashes onbenches, tables, or floors.

• Dispose of all unlabeled and contaminatedchemicals IAW local environmental regulations orSOPs.

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Figure 10-1. Preparation of a carboy for storage of acidic and basic solutions

Handling Chemicals. To prevent personal in-jury and damage to surrounding areas while han-dling chemicals, the following measures should beemployed.

• Always pour acid into water, especiallysulfuric acid. Never pour water into acid.

• Use Pyrex glassware when diluting acids.Ordinary glassware may be broken by the heatgenerated from the mixture of acid and water.

• Never heat mercury in an open containerand never shake more than 20 millimeters of mer-cury in a glass container. If a spill occurs, ensureadequate ventilation.

• Hold the container cap in your free handwhen pouring a sample from a container or bottle.Never place the cap or stopper on a counter, as itmay contaminate the sample. Clean up the mer-cury and sulfur together and put them in a suitablecontainer for disposal IAW local environmentalregulations.

• If any chemical is spilled or splashed onthe body, immediately wash the contaminated areathoroughly with water.

• If a strong solution of tetraethyl lead isspilled, cover the spill with dry chloride of lime,CaOC12 … Sand or other noncombustible absorb-ent material may also be used. Wait 5 minutes forreaction to be completed. Flush off with waterand wash area with soap and water. If the solu-tion is spilled on clothing, remove clothing and dis-card contaminated articles. Do not attempt towash contaminated clothing for reuse. Collect allcontaminated absorbent materials and place theminto a suitable container for disposal IAW localenvironmental regulations or SOPs. Contact thelocal environmental office for further guidance onspill reporting, cleanup, and disposal procedures.

• Make certain that a supply of dilute (18%)acetic acid is available when a doctor test or alkaliwash is being performed. Use the dilute acidfreely on any part of the body, except the eyes,

that may be contaminated with doctor or causticsolution. If doctor or caustic solution should con-taminate the eyes, immediately wash out withwater and report to hospital.

WARNING: Mercury is a poisonous materialthat may enter the body by ingestion, inhalation, orskin absorption. Mercury has such density, highsurface tension, and low viscosity that pouringwithout splashing and spilling is almost impossible.When mercury is poured, always use a funnel andmake the transfer over spill trays. If a mercuryspill occurs, make sure there is adequate ventila-tion. Do not vacuum or sweep the area as this willdisperse mercury throughout the laboratory.Cover the spill with sulfur. Clean up the mercuryand sulfur together and discard them in a suitablecontainer. All spills must be reported to the localenvironmental office.

SUBSTITUTE SOLVENTS

Field conditions may require the substitutionof certain solvents. In this case, the commonsenserule of "like dissolves like" should be used. Whenin doubt as to the correct solvent to substitute,consult the ASTM test method. For example,toluene could possibly be substituted for benzene ina solvent capacity, but n-hexane would not servethe purpose.

HANDLING EXCESS CHEMICALS

Contaminated chemicals are useless. Do notplace spatulas and other objects in chemical con-tainers, as the spatula may contain foreign matterthat will cause contamination. Similarly, if excesschemicals or samples are removed from a con-tainer, do not put it back into the container. All

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used chemicals should have well-established rulesfor disposal.

HANDLING SOLUTIONS

Prepare a chromic acid cleaning solution byslowly adding 800 milliliters of concentrated sulfu-ric acid to 500 milliliters of a saturated solution ofpotassium di chromate and water. Prepare thesolution in a sink, using a Pyrex container orequivalent glassware. Although chromic acid is

more effective as a cleaning agent when it isheated, precaution should be taken to avoid boilingthe solution. If the solution develops a greenishcolor, it is useless and should be discarded.

WARNING: Handle the solution with extremecare to avoid personal injury. A face shield andrubber gloves should be used. Chromic acid is apowerful oxidizing agent.

To increase the rate of solution, use a hot-plate, not an open flame. Heat the solution in aPyrex container or equivalent glassware under afume hood. If a water-free solution is not neces-sary, dissolve the solute in a small quantity of wa-ter before adding it to the warm alcohol.(Alcoholic solutions have toxic and flammableproperties.)

WARNING: Never use high-temperature ovensto heat volatile fluids. An explosion may occurand injure personnel.

CONTROLLING PRESSURE ANDVACUUM

The following safety precautions should beobserved by all personnel while operating theair/vacuum systems.

• Handle cylinders of compressed gas withparticular care. Never allow cylinders to drop orbounce or to come in contact with fire, sparks, orelectrical circuits, as explosions may result.

(Because compressed-gas cylinders are made ofsteel, such explosions have the same destructiveeffect as a bomb burst.)

• Make sure that all store cylinders arecapped, are supported to prevent rolling or falling,and are stored away from heat.

• Always store and transport cylinders in anupright position.

• Never put oil or grease on the valves ofcylinders or pressure regulators (pressurized oxy-gen and oil can create an explosion).

• Do not exceed the pressure or tempera-ture that has been designated as the safe upperlimit for

the apparatus or equipment being used, Do notuse a cylinder without a regulator.

• Do not use faulty copper, plastic, or rubbertubing when performing operations requiring pres-sure or vacuum.

• Make sure that glass vacuum apparatus isproperly shielded when it is in use.

• Release pressure cautiously when usinggasoline bombs for tests. The bomb plug maystick momentarily and then blow out suddenly.

• Always wear goggles when opening airvalves that are close to the face.

• Store propane cylinders in the propanestorage locker, away from heat or ignition sources.

The following safety precautions should beobserved by all personnel handling chemical con-tainers.

• Make sure that chemical containers hav-ing vent caps are inspected, and containers that donot have vent caps are vented periodically.

• Keep containers of volatile liquids as coolas possible. Exercise caution in releasing anypressure that may have formed in the container.Always release the pressure gradually.

• Remove caps or stoppers periodically tovent the vapor. (The practice of venting contain-ers of volatile liquids does not apply to those sam-ples collected for vapor pressure tests.)

• Vent separator funnels frequently whenshaking volatile liquids. Always wrap the funnel

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with a rag when shaking an extremely volatile liq-uid.

Other laboratory equipment that requires safehandling procedures are discussed below.

• Glassware. Wash the apparatus with sol-vent, soapy water, tap water, or distilled water,and then allow to dry. If necessary use a cleaningsolution. When glassware is prepared for storage,the stopcocks should be free of grease. StoreTeflon stopcocks, or their equivalent, loosely in thebarrel and keep them free of grease. Wrap glassstopcocks with a strip of paper for long-term stor-age to avoid fusing of surfaces such as glass stop-pers in flasks.

• Crucibles. Mark crucibles permanently

with ink manufactured for this purpose. India inkor pencil markings cannot withstand the high tem-perature crucibles may be exposed to and cannotbe used for this purpose.

• Pipets. Before using, inspect pipets fordamage to the tip. Use a suction bulb, not themouth, to draw the liquid up to a point above theetched line. Remove the bulb and rub thumbacross the orifice, letting the meniscus drop to aposition where its lowest point coincides with theetched line. Touch the tip to a smooth surface toremove any remaining drop. Allow liquid to draininto an appropriate container. Touch the tip to theside of the glass to ensure complete drainage.Pipets marked TD should not have the remainingdrops blown out upon drainage.

• Spatulas. Use steel spatulas only whennecessary. A small, clean sheet of paper will of-ten serve the same purpose and can be disposedof after use.

• Centrifuge and Centrifuge Tubes. Do notopen the centrifuge enclosure while the centrifugeis in operation. Centrifuge tubes positioned oppo-site each other must not differ in weight by morethan 1 gram.

• Separatory funnels. Hold separatory fun-nels with the palm of the left hand, securing thestopper firmly in place. Use the right hand to op-erate the stopcock. When the stopcock is openedfor venting, the outlet should be directed away

from the operator for safety reasons. Remove thestopper for rapid drainage.

• Corks. Bore corks on a soft wood surfaceafter softening the cork with a roller. When in-serting glass tubing or thermometers into corks,wrap the glass in a cloth and hold it as near to thecork as possible. Use water or glycerin as a lubri-cant. Fire-polish edges of glass tubing to avoidinjury to laboratory personnel. Use corks in pref-erence to rubber stoppers because corks are eas-ier to bore and are less reactive.

• Thermometers. The mercury in ther-mometers may contain bubbles. To remove thebubbles, carefully heat the bulb so that the mer-cury line slowly extends the length of the instru-ment; then slowly cool the thermometer.

• Ventilation and Fume Hoods. Make surethat the laboratory is ventilated adequately and thatfume hoods are operating properly. Use fumehood when working with toxic vapors. Leave thearea immediately if a material that gives off toxicvapors is spilled. Return to the area only after ithas been ventilated, or if fresh-air respirators havebeen obtained.

CONTROLLING FUMES

The following safety precautions are pre-sented to aid in controlling toxic fumes.

• Make sure the laboratory is properly ven-tilated and the fume hoods are operating properly.The supply room, where chemicals are stored,must also be adequately ventilated.

• Always work in a fume hood when usingbenzene, aniline, bromine water, or other materialsproducing toxic vapors.

• Perform all gas alarm system tests andcalibrations as specified to ensure proper operationof system.

• If any material is spilled which gives offtoxic fumes, all personnel should leave the areaimmediately and return only after the area hasbeen adequately purged, or after suitable breathingequipment has been obtained.

ELECTRICAL SAFETY

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The following electrical safety precautionsapply to all operators and maintenance personnelfor the petroleum laboratories.

• Equipment producing a tingle sensationshould be reported promptly for repair.

• Keep the use of extension cords to aminimum and the cords as short as possible.

• Be sure insulation and wire size are ade-quate for the voltage and current to be carried.

• Work on electrical devices should be doneafter the power has been disconnected or shut off,and suitable precautions taken to keep the poweroff during the work.

• If it is necessary to work on “live” electri-cal equipment, the person doing so must be fullyknowledgeable and have a second person presentwho is trained in first aid. Never work on “live”equipment alone.

• Wear safety glasses or a face shieldwhere sparks or arcing may occur.

• Never use metallic pencils or rulers, orwear rings or watches when working on electricalequipment.

• Avoid using or storing flammable liquidsnear electrical equipment.

Section II. Laboratory Analysis Reporting

GENERAL

Laboratory administrative procedures dis-cussed in this section are not mandatory. They areincluded only as suggested methods of accountingfor samples received for the following purposes:

• Testing.• Initiating the analysis reports.• Assigning routine and special tests to

laboratory technicians.• Recording test results.• Reporting test results to requesting agen-

cies with recommendations for use, reclamation,downgrading, or other disposition.

PETROLEUM SAMPLE TAG FILE

The petroleum sample tag should be detached(at the perforation) from the sample container atthe time of receipt. The laboratory number is as-signed serially from the laboratory logbook, andpreliminary information about the sample is re-corded in the logbook. This information includesthe sample number, date sampled, unit submittingsample, laboratory number, grade of product,specification, source of sample, quantity repre-sented, date received, date test started, date testcompleted, and remarks.

PETROLEUM LABORATORY ANALYSISREPORT

Recording Analyses. The senior laboratorytechnician transfers information on the sample tagto the heading of a DA Form 2077 (see Figure 10-2). The sample tag is then returned to the cardfile.

The technician refers to the product specificationto determine the tests to be performed and recordslimits on the DA Form 2077 work copy. He thensends this information by informal memorandumsto the technicians. The memorandums are identi-fied by the laboratory number of the analysis re-port. Work copies of all analysis reports in processare arranged by laboratory report number and at-tached to a clip board kept in a central location.Notebooks may be kept by laboratory techniciansto record test data. When a test or a series ofidentical tests are completed, the technicians turnin results to the senior technician. The senior tech-nician reviews each complete work copy for com-pletion of required tests and test accuracy. Theresults are recorded on the work copy. He thenmakes a recommendation for disposition and givesit to the laboratory NCOIC for review/approval.The NCOIC reviews the test results, comparesthem with use limits for the product, and decides

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whether the product represented by the samplecan be safely used for its intended purpose. If alluse limits have been met, the product is approvedfor use. The approval is indicated on the bottom ofthe report with or without a time limitation, as ap-propriate.

Processing. A typed report is prepared fromthe approved work copy. The senior techniciansends the report, including enough copies to satisfy

interested agencies, to the requesting agency. Thetechnician also provides a copy for the laboratory.The original is forwarded to the requesting agency.A carbon copy of the typed report, the work copy,and the sample tag are fastened together andplaced in a permanent file for future reference.

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Figure 10-2. DA Form 2077

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Recommendations for Disposition. If theproduct should not be used for its intended pur-pose, an alternative use must be considered andsuitable recommendations made. The report shouldinclude the following information:

• Probable cause of product not meeting uselimits.

• Nature and probable cause or source ofcontamination.

• Suggestions for preventing future con-tamination or deterioration.

• Recommendations for reclamation orother disposition of the product.

• On grade—Sample meets all specificationrequirements and can be retained for long storage.

• Suitable for use—Product is either dete-riorated or contaminated to the point where one ormore tests do not meet specification requirementsbut meet use limits (MILHDBK-200). Productshould be used as soon as possible.

• Not suitable for use—Product fails tomeet one or more use limits or specification re-quirement that has no use limit. Product must bedowngraded or blended as recommended andretested before use.

TESTING

Correlation Testing. Correlation testing maybe done by sending identical samples to two ormore laboratories. These laboratories use thesame apparatus in performing the tests. Correla-tion testing may also be done by having two ormore technicians within a given laboratory performtests on identical samples using the same appara-tus under controlled conditions. Another way oftesting is to have a single technician perform dupli-cate tests on identical material using the same ap-paratus under controlled conditions. Results shouldnot differ by more than those specified in the testmethod. The first two procedures are checks onreproducibility, the third is a check on repeatability.

Equipment Calibration. Results of all testsare dependent on calibrated equipment. MostArmy

equipment requiring calibration is listed in TB 43-180. Also, the calibration frequency and standardfor test equipment is specified in the applicable testmethods. Internally, the laboratory should verifycalibration more frequently than TB 43-180 re-quires.

• C-level calibration procedures. C-levelcalibration will be performed by qualified labora-tory personnel assigned to the laboratory.

• Analytical balance. The electric balance isa single-arm balance and has a weighing capacityof 100 grams. When the balance is provided withthe manual taring accessories, the weighing ca-pacity is increased to 150 grams. The precision(standard deviation) of the balance is plus or minus0.05 milligrams; digital readability is 0.1 milligrams;and accuracy in the optical range is plus or minus0.05 milligrams. ASTM E 319 procedures are rec-ommended for evaluating performance and veri-fying the accuracy of the balance. These proce-dures determine the precision that a balance cancompare known weight loads; that is, the built-inweights of the balance and a known weight load.Section 5, ASTM E 319, outlines procedures forpreparing the balance for evaluation and section 8outlines procedures for evaluating balance accu-racy. A precision weight set (class S) is used toevaluate balance performance. The verificationand evaluation of the balance are performed byoperating personnel. The double beam balancemay be evaluated using the above procedures. Thestandard deviation of the double balance is plus orminus 0.1 grams.

• Manometer. The manometer is used toverify the accuracy of the RVP gauges. Mercuryis used as the indicating fluid. The manometer isequipped with a double scale graduated in inchesof mercury and psi. The scale has provisions forzero adjustment. The scale must be adjusted to thezero position prior to verifying gage accuracy. Theaccuracy of the manometer is verified by using acertified master gage with a range of zero to 15psi graduated in increments of 0.1 psi and an accu-racy of plus or minus 0.05 percent. RecommendedA-level calibration frequency is 180 days.

• RVP gages. The RVP gages must beverified for accuracy after each test when deter-

FM 10-67-2

10-13

mining vapor pressure of MOGAS. When deter-mining the vapor pressure of aviation fuels(AVGAS and turbine engine fuel), operating per-sonnel verify the gage for accuracy before andafter each test. The accuracy of RVP gages isverified by using the manometer. When the gagereading and the manometer reading differ by 1percent or less; that is, the gage correction factoris not greater than 0.05 psi for 5-pound gages or0.15 psi for 15-pound gages, the gage is consid-ered accurate. However, if the readings differ bymore than 1 percent, the gauge is considered inac-curate and must be repaired or replaced.

• Thermometers. The routine laboratorythermometers, ASTM 9 F, 12 F, and 58 F, have

scales including 32°F and are verified for accu-racyby determining the ice point. ASTM 18 F is veri-fied at 100°F. ASTM 7 F, low distillation ther-mometer, is verified for accuracy at 200°F.ASTM 10 F, high range thermometer, is verifiedfor accuracy at 212°F. ASTM 7 F, 10 F, and 18F are verified for accuracy by direct comparisonwith a certified precision thermometer. The twocertified precision thermometers (ASTM 64 F and68 F) are certified by the A-level calibration facil-ity. The precision thermometers must be certifiedat 360-day intervals. The error of the certifiedthermometers must not be more than the maxi-mum scale error of the specification (ASTM E-1).

Section III. Standard Publications and Forms

GENERAL

Publications that describe the acceptablemilitary procedures for testing and evaluating thequality of a petroleum product are essential for usein a petroleum laboratory. The latest editions, withall change notices and current petroleum productspecifications, must be on hand at all times to beused by laboratory personnel.

MILITARY STANDARDIZATIONHANDBOOK FOR FUELS, LUBRICANTS,

AND RELATED PRODUCTS(MIL-HDBK-200)

This handbook provides general instructionsand minimum procedures to be used worldwide bythe military services in QS of US government-owned fuels, lubricants, and related products. Theprocedures described in MIL-HDBK-200 includeQS testing and use limits, minimum sampling andtesting requirements, types of tests required onvarious petroleum products, and storage and trans-portation requirements.

FEDERAL TEST METHODSTANDARD NO. 791

FTMS No. 791 covers methods adopted foruse by federal agencies in testing lubricants, liquidfuels, and related products. Only the federal testmethods without adopted ASTM test standardsare included in the publication. The federal stan-dard has both alphabetic and numeric indexes oftest methods. These list both the federal test des-ignation and the corresponding ASTM test desig-nation. New and revised federal test material andcancellation are issued as change notices by theGeneral Services Administration. These are num-bered consecutively and dated. Laboratoriesshould retain all change notices until superseded bya reissue of the entire federal standard.

ASTM STANDARDS 23, 24, 25, AND 47

FM 10-67-2

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The ASTM standards 23, 24, 25, and 47 arepublished annually and contain test methods forpetroleum products.

DFSCH 4120.1, REFERENCE LIST OFSPECIFICATIONS AND STANDARDS

This list shows all current petroleum specifi-cations and is published periodically by the De-fense Fuel Supply Center.

DOD MANUAL 4140.25-M, PROCEDURESFOR THE MANAGEMENT OF

PETROLEUM PRODUCTS

This manual covers procedures for manage-ment of DOD-owned petroleum stock.

AR 715-27 (DLAM 4155.1), PETROLEUMPROCUREMENT QUALITY ASSURANCE

MANUAL

This manual covers all areas of petroleumQA.

FORMS

The following forms may be used in a petro-leum laboratory.

• DA Form 285 (US Army Accident Inves-tigation Report.

• DA Form 1804 (Petroleum Sample). SeeFigure 9-4.

• DA Form 2077 (Petroleum ProductsLaboratory Analysis Report). See Figure 10-2.

• DA Form 2404 (Equipment Inspection andMaintenance Worksheet).

• DA Form 2407 (Maintenance Request).• DD Form 250 (Material Inspection and

Receiving Report). See Figure 10-3.• DD Form 250-1 (Material Inspection and

Receiving Report - Continuation Sheet). See Fig-ure 10-4.

• DD Form 314 (Preventive MaintenanceSchedule and Record).

• DD Form 1425 (Specifications and Stan-dards Requisition).

• SF 361 (Discrepancy in Shipment Report).

FM 10-67-2

10-15

MATERIAL INSPECTION AND RECEIVING REPORT

23. CONTRACTOR USE ONLY

1 9130-00-031-5816 Turbine Fuel, Aviation,

Grade JP-8, Kerosene type, MIL-T-83133 0

7. PAGE

1

* I f q u a n t i t y r e c e i v e d b y t h e G o v e r n m e n t i s t h es a m e a s q u a n t i t y s h i p p e d , i n d i c a t e b y (

4. B/L

2 0 .

A M O U N T

1 8 .

U N I T

bbl

1 6 . STOCK/PART NO. DESCRIPTION

( I n d i c a t e n u m b e r o f s h i p p i n g c o n t a i n e r s - t y p e o f c o n t a i n e r - c o n t a i n e r n u m b e r . )

A . ORIGIN

1 5 .

I TEMNO.

Public reporting burden for this collection of information is estimated to average 30 minutes per response, including the time for reviewing instructions, searching existing data sources, gathering andmaintaining the data needed, and completing and reviewing the collection of information. Send comments regarding this burden estimate or any other aspect of this collection of information,including suggestions for reducing this burden, to Department of Defense, Washington Headquarters Services, Directorate for Information Operations and Reports, 1215 Jefferson Davis Highway,Suite 1204, Arl ington, VA 22202-4302, and to the Off ice of Management and Budget, Paperwork Reduction Project (0704-0248), Washington, DC 20503.

1. PROC. INSTRUMENT IDEN. (CONTRACT) DSA-owned stock

6. INVOICE NO./DATE

2. SHIPMENT NO. 00012

5. DISCOUNT TERMS

DD Form 250 , NOV 92 USAPPC V2.00

Form Approved O M B N o . 0 7 0 4 - 0 2 4 8

8. ACCEPTANCE POINT

S(ORDER) NO.

3. DATE SHIPPED 30 Aug XX

TCN AZ40ZZ81930044XXX

13. SHIPPED TO TANK FARM

209TH SUPPLY CO

APO AE 09227

11. SHIPPED FROM (If other than 9)

BULK STORAGE FACILITY

APO AE 09345

FOB:

14. MARKED FOR

12. PAYMENT WILL BE MADE BY

10. ADMINISTERED BY 9. PRIME CONTRACTOR

P r e v i o u s e d i t i o n m a y b e u s e d .

1 9 .

UNIT PRICE

1 7 .

Q U A N T I T YS H I P / R E C ' D *

5,000

C O N T R A C T Q U A L I T Y A S S U R A N C E2 1 . 2 2 . RECEIVER'S USE

Q u a n t i t i e s s h o w n i n c o l u m n 1 7 w e r e r e c e i v e din appa ren t good cond i t i on excep t as no ted .

DATE RECEIVED SIGNATURE OF AUTH GOVT REP

TYPED NAME

AND OFFICE

B. DESTINATION

has been made by me o r unde r my supe r -

v i s i o n a n d t h e y c o n f o r m t o c o n t r a c t , e x c e p tas no ted he re in o r on suppor t i ng documen ts .

C Q A ACCEPTANCE o f l i s t ed i t ems C Q A ACCEPTANCE o f l i s t ed i t emsh a s b e e n m a d e b y m e o r u n d e r m y s u p e r v i s i o n a n d

t h e y c o n f o r m t o c o n t r a c t , e x c e p t a s n o t e d h e r e i no r o n s u p p o r t i n g d o c u m e n t s .

TYPED NAME

AND OFFICE

TYPED NAME

AND TIITLE

CODE

CODE

CODE

CODE

CODE

CODE

DATE SIGNATURE OF AUTH GOVT REPDATE SIGNATURE OF AUTH GOVT REP

1OF

i f d i f f e r e n t , e n t e r a c t u a l q u a n t i t y r e c e i v e d b e l o wq u a n t i t y s h i p p e d a n d e n c i r c l e .

) m a r k ,

PLEASE DO NOT RETURN YOUR COMPLETED FORM TO E ITHER OF THESE ADDRESSES. S E N D T H I S F O R M I N A C C O R D A N C E W I T H T H E I N S T R U C T I O N S C O N T A I N E D I N T H E D F A R S , A P P E N D I X F - 4 0 1 .

Figure 10-3. DD Form 250

FM 10-67-2

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Figure 10-4. DD Form 250-1