ASTM Oxygen Cleaning MIL-STD-1330D - CHG-1
ASTM Oxygen Cleaning MIL-STD-1330D - CHG-1
ASTM Oxygen Cleaning MIL-STD-1330D - CHG-1
com
INCH-POUND
MIL-STD-1330D(SH)
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28 June 2007
SUPERSEDING
MIL-STD-1330D(SH)
20 September 1996
DEPARTMENT OF DEFENSE
STANDARD PRACTICE
MIL-STD-1330D(SH)
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FOREWORD
1. This standard is approved for use by the Naval Sea Systems Command, Department of the Navy, and is
available for use by all Departments and Agencies of the Department of Defense.
2. This standard is for use by naval activities and private firms performing services as prime or sub-
contractors for Naval Sea Systems Command.
3. Comments, suggestions, or questions on this document should be addressed to Commander, Naval Sea
Systems Command, ATTN: SEA 05Q, 1333 Isaac Hull Avenue, SE, Stop 5160, Washington Navy Yard, DC 20376-
5160 or emailed to [email protected], with the subject line “Document Comment”. Since contact
information can change, you may want to verify the currency of this address information using the ASSIST Online
database at http://assist.daps.dla.mil.
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CONTENTS
PARAGRAPH PAGE
1. SCOPE.......................................................................................................................................................... 1
1.1 Scope .......................................................................................................................................................... 1
1.2 Applicability ............................................................................................................................................... 1
3. DEFINITIONS ............................................................................................................................................. 6
3.1 Aqueous cleaning solution.......................................................................................................................... 6
3.2 Blue line...................................................................................................................................................... 6
3.3 Clean........................................................................................................................................................... 6
3.4 Cleaning solvent ......................................................................................................................................... 6
3.5 Cleanliness level ......................................................................................................................................... 6
3.6 Clean lint-free cloth .................................................................................................................................... 6
3.7 Cleanroom .................................................................................................................................................. 6
3.8 Components ................................................................................................................................................ 6
3.9 Contractor ................................................................................................................................................... 6
3.10 Controlled area ......................................................................................................................................... 6
3.11 Critical applications .................................................................................................................................. 6
3.12 Dew point ................................................................................................................................................. 6
3.13 Final cleaner ............................................................................................................................................. 6
3.14 Halogenated solvent ................................................................................................................................. 7
3.15 Helium ...................................................................................................................................................... 7
3.16 Maximum operating pressure ................................................................................................................... 7
3.17 Membrane filter ........................................................................................................................................ 7
3.18 Nitrogen.................................................................................................................................................... 7
3.19 Objective quality evidence ....................................................................................................................... 7
3.20 Organic ..................................................................................................................................................... 7
3.21 Oxygen clean ............................................................................................................................................ 7
3.22 Oxygen enriched....................................................................................................................................... 7
3.23 Precision cleaning..................................................................................................................................... 7
3.24 Pre-cleaner ................................................................................................................................................ 7
3.25 Sample ...................................................................................................................................................... 7
3.26 Surfactant.................................................................................................................................................. 7
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CONTENTS - Continued
PARAGRAPH PAGE
3.27 Validation ................................................................................................................................................. 7
3.28 Vendor ...................................................................................................................................................... 7
3.29 Water ........................................................................................................................................................ 8
3.30 Wetted surface .......................................................................................................................................... 8
4. GENERAL REQUIREMENTS.................................................................................................................... 8
4.1 Oxygen safety precautions.......................................................................................................................... 8
4.2 Water .......................................................................................................................................................... 8
4.2.1 Applicability ............................................................................................................................................ 8
4.2.2 Disposal ................................................................................................................................................... 8
4.2.3 Compatibility ........................................................................................................................................... 8
4.3 Aqueous cleaning solutions ........................................................................................................................ 8
4.3.1 Navy oxygen cleaner (NOC) ................................................................................................................... 8
4.3.2 Tribasic sodium phosphate (TSP)............................................................................................................ 11
4.3.3 Non-ionic detergent (NID) ...................................................................................................................... 12
4.4 Cleaning solvents........................................................................................................................................ 12
4.4.1 NAVSEA approved halogenated solvents ............................................................................................... 12
4.4.2 Isopropyl alcohol ..................................................................................................................................... 14
4.5 Other cleaners ............................................................................................................................................. 14
4.5.1 Other pre-cleaners.................................................................................................................................... 14
4.5.2 Other final cleaners.................................................................................................................................. 15
4.6 Incompressible test fluids ........................................................................................................................... 15
4.6.1 Safety precautions.................................................................................................................................... 15
4.6.2 Water ....................................................................................................................................................... 15
4.6.3 Cleaning solvent ...................................................................................................................................... 15
4.7 Compressible test fluids.............................................................................................................................. 15
4.7.1 Safety precautions.................................................................................................................................... 15
4.7.2 Helium ..................................................................................................................................................... 15
4.7.3 Nitrogen................................................................................................................................................... 15
4.7.4 Oxygen .................................................................................................................................................... 15
4.7.5 Argon....................................................................................................................................................... 15
4.8 Cleaning silver-brazed piping..................................................................................................................... 16
4.9 Lubricants ................................................................................................................................................... 16
5. DETAILED REQUIREMENTS................................................................................................................... 16
5.1 Facility requirements .................................................................................................................................. 16
5.1.1 Structure .................................................................................................................................................. 17
5.1.2 Maintenance............................................................................................................................................. 17
5.1.3 Temperature and humidity....................................................................................................................... 18
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CONTENTS - Continued
PARAGRAPH PAGE
5.1.4 Air filtration............................................................................................................................................. 18
5.1.5 Ventilation and air pressure ..................................................................................................................... 18
5.1.6 Personnel clothing ................................................................................................................................... 18
5.1.7 Tools and equipment................................................................................................................................ 19
5.2 Aqueous component cleaning process ........................................................................................................ 19
5.2.1 Applicability ............................................................................................................................................ 19
5.2.2 Objective.................................................................................................................................................. 19
5.2.3 Material and equipment ........................................................................................................................... 19
5.2.4 Pre-clean and rinse................................................................................................................................... 20
5.2.5 Final clean, verification, and rinse........................................................................................................... 20
5.2.6 Dry, reassemble, and package.................................................................................................................. 21
5.3 Flask cleaning and inspection ..................................................................................................................... 21
5.3.1 Applicability ............................................................................................................................................ 21
5.3.2 Material and equipment ........................................................................................................................... 21
5.3.3 Clean, verification, and rinse ................................................................................................................... 21
5.3.4 Drying...................................................................................................................................................... 22
5.3.5 In-service interior inspection ................................................................................................................... 22
5.4 Cleaning and calibration of instruments and gauges .................................................................................. 23
5.5 Aqueous system cleaning process............................................................................................................... 23
5.5.1 Applicability ............................................................................................................................................ 23
5.5.2 Material and equipment ........................................................................................................................... 23
5.5.3 System preparation .................................................................................................................................. 23
5.5.4 Electrolytic oxygen gas generators .......................................................................................................... 24
5.5.5 Leak-check............................................................................................................................................... 24
5.5.6 Preflush.................................................................................................................................................... 24
5.5.7 Hydrostatic test ........................................................................................................................................ 24
5.5.8 Final flush or pipe line cleaning .............................................................................................................. 24
5.5.9 Rinsing and particulate flushing .............................................................................................................. 25
5.5.10 Drying and reinstalling components ...................................................................................................... 26
5.6 Potassium hydroxide (KOH) inspection ..................................................................................................... 26
5.6.1 Applicability ............................................................................................................................................ 26
5.6.2 Inspection ................................................................................................................................................ 26
5.6.3 KOH removal .......................................................................................................................................... 26
5.7 Flushing of ships service demineralized water piping systems .................................................................. 26
5.7.1 Applicability ............................................................................................................................................ 26
5.7.2 Material and equipment ........................................................................................................................... 27
5.7.3 Flush ........................................................................................................................................................ 27
5.7.4 Visual inspection .................................................................................................................................... 27
5.8 Solvent system cleaning processes ............................................................................................................. 27
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CONTENTS - Continued
PARAGRAPH PAGE
5.8.1 Applicability ............................................................................................................................................ 27
5.8.2 Oxygen-nitrogen plants ........................................................................................................................... 27
5.8.3 Oxygen-nitrogen plant piping.................................................................................................................. 28
5.9 Testing ........................................................................................................................................................ 29
5.9.1 Pressure testing ........................................................................................................................................ 29
5.9.2 Operational testing................................................................................................................................... 31
5.9.3 Gas sampling and analysis....................................................................................................................... 31
5.10 Removal and replacement of components in oxygen clean systems ........................................................ 32
5.10.1 General requirements............................................................................................................................. 32
5.10.2 Purge...................................................................................................................................................... 33
5.11 Piping repairs............................................................................................................................................ 34
5.11.1 Applicability .......................................................................................................................................... 34
5.11.2 System preparation ................................................................................................................................ 34
5.11.3 Maintenance of purge ............................................................................................................................ 34
5.11.4 Cutting or grinding of system ................................................................................................................ 34
5.11.5 Cleaning................................................................................................................................................. 34
5.11.6 Inspection and testing ............................................................................................................................ 34
5.12 Loss of system cleanliness........................................................................................................................ 34
5.12.1 Definition............................................................................................................................................... 34
5.12.2 Method for determination of extent of contamination ........................................................................... 34
5.12.3 Corrective action.................................................................................................................................... 35
5.12.4 Local cleaning........................................................................................................................................ 35
5.13 Process verification methods .................................................................................................................... 35
5.13.1 Visual surface inspection methods ........................................................................................................ 35
5.13.2 Hydrocarbon and NVR analysis methods.............................................................................................. 36
5.13.3 Particulate inspection methods .............................................................................................................. 37
5.13.4 pH analysis ............................................................................................................................................ 37
5.13.5 NOC alkalinity....................................................................................................................................... 38
5.13.6 Detection of hydrocarbon contamination by swipe ............................................................................... 39
5.14 Personnel qualification and training ......................................................................................................... 39
5.14.1 Applicability .......................................................................................................................................... 39
5.14.2 Course of instruction.............................................................................................................................. 40
5.14.3 Requalification....................................................................................................................................... 40
5.15 Validation of the component cleaning process ......................................................................................... 40
5.15.1 Periodicity.............................................................................................................................................. 40
5.15.2 Procedure ............................................................................................................................................... 40
5.16 Packaging, identification, and storage ...................................................................................................... 40
5.16.1 Packaging............................................................................................................................................... 40
5.16.2 Identification.......................................................................................................................................... 42
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CONTENTS - Continued
PARAGRAPH PAGE
5.16.3 Storage................................................................................................................................................... 42
5.17 In-process inspections............................................................................................................................... 42
5.17.1 Inspection............................................................................................................................................... 42
5.17.2 Objective quality evidence (OQE)......................................................................................................... 42
5.17.3 Audit or surveillance.............................................................................................................................. 42
5.17.4 Accountability of small items ................................................................................................................ 44
6. NOTES ......................................................................................................................................................... 44
6.1 Intended use................................................................................................................................................ 44
6.2 Acquisition requirements............................................................................................................................ 44
6.3 NAVSEA approval and direction ............................................................................................................... 44
6.4 Safety precautions....................................................................................................................................... 45
6.5 Subject term (key word) listing .................................................................................................................. 45
6.6 Change notations ........................................................................................................................................ 45
FIGURES
1. Typical certification sticker .......................................................................................................................... 45
2. Typical certification tag................................................................................................................................ 46
3. Filtration for determining NVR in NOC by gravimetric .............................................................................. 56
4. Cross-sectional view of evaporating dish ..................................................................................................... 62
5. 5 PPM acceptance criteria for sample........................................................................................................... 74
TABLES
I. Grades of water ............................................................................................................................................. 8
II. Cleanroom and controlled area requirements............................................................................................... 16
III. Applicability matrix for flush duration and back flush............................................................................... 25
IV. Solvent cleaning processes ......................................................................................................................... 27
V. Hydrostatic testing ....................................................................................................................................... 29
VI. Joint tightness testing ................................................................................................................................. 30
VII. Seat tightness testing ................................................................................................................................. 31
VIII. Pressure drop testing................................................................................................................................ 31
IX. Containment and purge requirements......................................................................................................... 32
X. Hydrocarbon and NVR analysis methods.................................................................................................... 36
XI. Film for packaging ..................................................................................................................................... 41
XII. In-process operation inspections ............................................................................................................... 43
A-I. Metallic material compatibility ................................................................................................................. 48
A-II. Rubber material compatibility ................................................................................................................. 49
A-III. Plastic material compatibility ................................................................................................................. 50
A-IV. Rubber compatibility criteria.................................................................................................................. 51
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CONTENTS - Continued
TABLES PAGE
A-V. Plastic compatibility criteria .................................................................................................................... 51
D-I. Preparation and analysis of 5 ppm equivalent laboratory standards.......................................................... 67
D-II. Dish acceptance criteria applicability matrix........................................................................................... 67
D-III. Acceptable range for 5 ppm acceptance criteria without baseline.......................................................... 70
D-IV. Acceptable range for 5 ppm acceptance criteria with baseline............................................................... 72
D-V. 5 PPM acceptance criteria for sample...................................................................................................... 74
E-I. NAVSEA approved halogenated solvents................................................................................................. 80
APPENDICES
A MATERIAL COMPATIBILITY.................................................................................................................. 47
B ANALYSIS OF NON-VOLATILE RESIDUE IN NAVY OXYGEN CLEANER BY GRAVIMETRIC... 52
C TEST PROCEDURE FOR SOLVENT EXTRACTION OF AN AQUEOUS INORGANIC CLEANER... 57
D ANALYSIS OF RESIDUE IN SOLVENT BY OPTICALLY STIMULATED ELECTRON
EMISSION USING A SURFACE QUALITY MONITOR.......................................................................... 60
E NAVSEA APPROVED HALOGENATED SOLVENTS ............................................................................ 80
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1. SCOPE
1.1 Scope. This standard provides the requirements for precision cleaning and testing of oxygen or oxygen-
enriched systems and components; oxygen generating plants including nitrogen, hydrogen, and demineralized water
support systems and components; and helium, helium-oxygen, and hydrogen life support systems and components.
Each activity will implement the applicable requirements of this document through a locally prepared and approved
procedure. Activities subject to additional quality assurance requirements such as NAVSEA SS800-AG-MAN-
010/P-9290 or NAVSEA SS521-AA-MAN-010 will obtain procedure approval from the applicable certifying
activity.
1.2 Applicability. This standard is applicable to all surface ships, submarines, and supporting shore base
facilities which contain any of the following:
1.2.1 Oxygen or oxygen-enriched systems and components, including gaseous and liquid oxygen generating
equipment. The cleanliness boundary includes all material wetted by any fluid containing greater than 25 percent by
volume oxygen during normal operations. An exception is the following diver life support equipment: diving
helmets, masks, umbilicals, and items otherwise exempt by NAVSEA which are cleaned in accordance with MIL-
STD-1622, critical applications. For information, compressed air systems directly supporting oxygen generating
equipment are cleaned in accordance with MIL-STD-1622, critical applications.
1.2.2 Hydrogen, nitrogen, and demineralized water systems and components that support gaseous or liquid
oxygen generating equipment.
1.2.2.1 The cleanliness boundary for hydrogen systems supporting oxygen generating equipment encompasses
all wetted material from, and including, the point of interface or interface connection with an oxygen or oxygen-
enriched system or component to the first check valve or normally shut isolation valve. Remaining portions of
hydrogen systems should be cleaned using best commercial practice to remove loose scale, dust, grit, filings, oil, and
grease.
1.2.2.2 The cleanliness boundary for submarine nitrogen systems supporting oxygen generating equipment
encompasses all wetted material from, and including, the point of interface or interface connection with an oxygen
or oxygen-enriched system or component upstream to either:
a. The nitrogen supply flasks, including all piping and components associated with charging when such
supply is dedicated to oxygen generating equipment. Nitrogen piping to the ship demineralized water storage tank is
cleaned in accordance with MIL-STD-1622, general applications.
b. The last check valve or normally shut isolation valve that separates the nitrogen supply flasks from the
oxygen generator when such supply is not dedicated to oxygen generating equipment. Remaining portions of the
nitrogen system are cleaned in accordance with MIL-STD-1622, general applications.
1.2.2.3 The cleanliness boundary for surface ship nitrogen systems includes any portion of the system that can
be used to pressurize or purge the oxygen system, oxygen system components, oxygen-nitrogen producer, and
storage equipment. Remaining portions of the nitrogen systems are cleaned in accordance with MIL-STD-1622,
general applications.
1.2.2.4 The cleanliness boundary for demineralized water systems supporting oxygen generating equipment
encompasses all wetted material from, and including, the point of interface or interface connection with an oxygen
or oxygen-enriched system or component to the ship’s demineralizer.
1.2.3 Helium, helium-oxygen, and hydrogen systems and components that provide life support. The cleanliness
boundary encompasses all wetted material providing life support functions except the following: diving helmets,
masks, umbilicals and items otherwise exempted by NAVSEA which are cleaned in accordance with MIL-STD-
1622, critical applications.
1.2.4 Equipment which comes in contact with or is used to transfer any fluid from its source to a system or
component within any of the boundaries defined in 1.2.1, 1.2.2, and 1.2.3 when such interface is intended to
maintain the cleanliness requirements specified herein.
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1.2.5 Open ended applications constructed of material that is configured and operated at a pressure that
represents a fire hazard in the presence of an oxygen or oxygen-enriched atmosphere when determined in
accordance with the guidelines of ASTM G63 and ASTM G94. For open-ended piping or configurations
constructed of material and operated in an oxygen or oxygen-enriched atmosphere at a pressure that does not
propagate a flame when determined in accordance with the guidelines of ASTM G63 and ASTM G94, clean in
accordance with MIL-STD-1622 for diver applications; otherwise use best commercial practice to remove loose
scale, dust, grit, filings, oil, and grease. For information, copper, copper-nickel, bronze, brass, and monel will not
propagate a flame in an oxygen or oxygen-enriched atmosphere at pressures up to 7500 pounds per square inch
(lb/in2).
2. APPLICABLE DOCUMENTS
2.1 General. The documents listed in this section are specified in sections 3, 4, or 5 of this standard. This
section does not include documents cited in other sections of this standard or recommended for additional
information or as examples. While every effort has been made to ensure the completeness of this list, document
users are cautioned that they must meet all specified requirements of documents cited in sections 3, 4, or 5 of this
standard, whether or not they are listed.
2.2 Government documents.
2.2.1 Specifications, standards, and handbooks. The following specifications, standards, and handbooks form a
part of this document to the extent specified herein. Unless otherwise specified, the issues of these documents are
those cited in the solicitation or contract.
FEDERAL SPECIFICATIONS
O-S-642 - Sodium Phosphate, Tribasic, Anhydrous; Dodecahydrate; and
Monohydrate; Technical
TT-I-735 - Isopropyl Alcohol
ZZ-G-710 - Gasket Material, Rubber 35 Durometer Hardness
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SAE INTERNATIONAL
SAE-AS8660 - Silicone Compound, NATO Code Number S-736 (DoD adopted)
(Copies of this document are available online at www.sae.org or from the SAE World Headquarters, 400
Commonwealth Drive, Warrendale, Pennsylvania, 15096-0001.)
2.4 Order of precedence. In the event of a conflict between the text of this document and the references cited
herein, the text of this document takes precedence. Nothing in this document, however, supersedes applicable laws
and regulations unless a specific exemption has been obtained.
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3. DEFINITIONS
3.1 Aqueous cleaning solution. An aqueous cleaning solution is a water based cleaner whose constituents are
soluble inorganic compounds such as silicates or phosphates or soluble organic compounds such as non-ionic
surfactant or combinations thereof. Examples of aqueous cleaning solutions include commercial detergents which
generally contain both soluble inorganic and organic compounds and Navy oxygen cleaner (NOC) which contains
only soluble inorganic compounds.
3.2 Blue line. When a cut for a pipe or fitting nears the inner wall, the outer surface turns blue which is
referred to as cutting to the blue line. The blue line results from oxidation caused by the reduced ability of the
thinned pipe or fitting to dissipate heat generated by the power tool cutting the surface.
3.3 Clean. Clean refers to the absence of scale, particulate, oil, and grease contaminants at a level below that
which adversely affects the operation or reliability of the component or system. The process of cleaning should not
affect the form, fit, or function of the item being cleaned.
3.4 Cleaning solvent. A cleaning solvent is any material that exhibits the capability to dissolve other
substances through chemical action and, for the purposes of this document, is 100 percent volatile. Examples
include halogenated solvents such as HCFC-141b which is non-flammable and hydrocarbon solvents such as
isopropyl alcohol (IPA) which is very flammable.
3.5 Cleanliness level. A cleanliness level is an established maximum allowable distribution of contamination
of a given size and quantity in a specified area or volume.
3.6 Clean lint-free cloth. A clean lint-free cloth in accordance with MIL-DTL-24671, or equal, is used for local
cleaning or wiping surfaces to evaluate loss of cleanliness. The cloth should be free of chemicals which could pose
a compatibility, flammability, or toxicity hazard considering the specific application.
3.7 Cleanroom. A cleanroom is a permanent area where a high degree of cleanliness is continuously achieved
by employing varying degrees of control and monitoring of environmental items such as ventilation, filtration,
temperature, humidity, pressure, personnel, clothing, and room maintenance. Refer to 5.1 for cleanroom
requirements.
3.8 Components. Components refer to items such as valves, fittings, gauges, regulators, and repair parts in the
systems.
3.9 Contractor. A contractor is any person not employed by the U.S. Navy performing services on-board ships
or at shore base facilities on components or systems defined by 1.2.
3.10 Controlled area. A controlled area is an area where a high degree of cleanliness is temporarily achieved
and maintained by the use of temporary boundaries, air filtration, and the enforcement of strict controls on personnel
access, operations, and area maintenance. Controlled areas are most often used for in-place maintenance and repair
of shipboard systems. Refer to 5.1 for controlled area requirements.
3.11 Critical applications. Critical applications are systems or components requiring more detailed cleanliness
and packaging requirements than generally specified because of unique operating parameters and environments. In
the past, some saturated diving systems have been classified as critical applications because of the increased toxicity
hazard associated with high partial pressure environments. Unless directed by NAVSEA or the Type Commander,
critical requirements may not be used.
3.12 Dew point. Dew point is the measure of dryness or wetness of a gas. It is defined as the temperature at
which gas becomes saturated with water vapor causing condensation when cooled at constant pressure. Dew point
temperature is measured at atmospheric pressure.
3.13 Final cleaner. A final cleaner is an aqueous cleaning solution or a cleaning solvent used for final flushing
of piping systems or final precision cleaning of components and parts.
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3.14 Halogenated solvent. A halogenated solvent is any solvent whose chemical structure contains bromine,
chlorine, fluorine, or iodine. Most halogenated solvents are non-flammable and many are very toxic. All NAVSEA
approved halogenated solvents contain fluorine, some also contain chlorine, and none contain bromine or iodine.
3.15 Helium. Helium refers to gaseous helium as specified in 4.7.2.
3.16 Maximum operating pressure. The maximum operating pressure is the highest pressure that can exist in a
system or subsystem under normal (non-casualty) operating conditions. This pressure is determined by such
influences as pressure regulating valve set pressure, maximum pressure at the system source such as compressed gas
bank pressure or sea pressure, and pump or compressor shut-off pressure for closed systems. For constant pressure
systems, such as regulated compressed gas systems, the term Nominal Operating Pressure has been used to designate
the steady state operating condition. Where this type of pressure rating is applied, for the purpose of the
requirements stated herein, it may be substituted as the maximum operating pressure.
3.17 Membrane filter. A membrane filter refers to an absolute rated filter where the filter retains all particles
whose smallest dimension is equal to or greater than the specified rating.
3.18 Nitrogen. Nitrogen refers to gaseous nitrogen as specified in 4.7.3.
3.19 Objective quality evidence. Objective quality evidence is any statement of fact, either quantitative or
qualitative, pertaining to the quality of a product or service based on observations, measurements, or tests which can
be verified. Evidence will be expressed in terms of specific quality requirements or characteristics. These
characteristics are identified in drawings, specifications, and other documents which describe the item, process, or
procedure.
3.20 Organic. Organic refers to any chemical compound containing carbon. For the purposes of this
document, the organic compounds of interest are hydrocarbon compounds containing carbon and hydrogen, and
fluorocarbon compounds containing carbon and fluorine. Hydrocarbon materials such as lubricating oils are very
flammable in oxygen, while fluorocarbon materials such as MIL-PRF-27617 grease demonstrate good compatibility
with oxygen.
3.21 Oxygen clean. Oxygen clean is the verifiable absence of particulate, fiber, oil, grease, and other
contaminants determined through the use of qualitative and quantitative cleanliness measurement techniques. An
oxygen, helium, helium-oxygen, nitrogen, nitrogen-oxygen, or hydrogen piping system or component successfully
cleaned in accordance with this standard is considered oxygen clean.
3.22 Oxygen enriched. Oxygen enriched refers to any fluid containing greater than 25 percent oxygen by
volume in accordance with ASTM G63 and ASTM G94.
3.23 Precision cleaning. Precision cleaning is the act of removing unwanted contaminants to better than visibly
clean. Precision cleaning is accomplished using a controlled and verifiable process with cleaning agents that satisfy
the applicable cleanliness requirements.
3.24 Pre-cleaner. A pre-cleaner is any aqueous cleaning solution or cleaning solvent used to clean parts to
visually clean. Examples include Navy oxygen cleaner (NOC), dissolved tribasic sodium phosphate (TSP),
isopropyl alcohol, and non-ionic detergent (NID) mixed with water or NOC or TSP.
3.25 Sample. Sample is a representative amount of cleaning solvent, cleaning solution, rinse water, or
pressurized gas collected in clean containers at selected locations obtained to verify the performance of the cleaning
process.
3.26 Surfactant. A surfactant is a surface wetting agent which reduces interfacial tension between a liquid and
a solid.
3.27 Validation. Validation is the demonstration of the ability to perform a technique or process with verifiable
results at a regular interval.
3.28 Vendor. A vendor is any person not employed by the U.S. Navy that performs services as specified in this
standard at a facility not owned or operated by the government.
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4.2.2 Disposal. Disposal of water shall be in accordance with local, state, and federal regulations.
4.2.3 Compatibility. Appendix A gives the compatibility of hot water with various materials. Where
incompatibility exists, process changes such as rinsing with cooler water, shorter rinse durations, or immediate
drying of wet surfaces may need to be considered. Where specific information is lacking, perform compatibility
testing as specified in A.3.1 of Appendix A.
4.3 Aqueous cleaning solutions.
4.3.1 Navy oxygen cleaner (NOC).
4.3.1.1 Applicability. NOC is an aqueous alkaline cleaning solution approved for use as a pre-cleaner or final
cleaner for all compatible piping and components other than liquid oxygen generating plants. It may be used for
liquid oxygen generating plant piping and components provided the aqueous cleaning process specified herein can
be successfully accomplished. NOC shall be in accordance with MIL-DTL-24800.
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4.3.1.2 Safety precautions. Follow the safety precautions recommended in the vendor’s material safety data
sheet (MSDS) and the following precautions recommended by the Navy Environmental Health Center (NEHC).
a. Skin contact with NOC will result in irritation and chemical burns. Wear impervious protection clothing
constructed of neoprene or other material of equivalent resistance to penetration so as to prevent skin contact. Use
elbow-length gloves (with cuffs) as minimum protection any time open containers of the cleaning agent are handled.
Wash potentially exposed skin areas with soap and water at breaks, and at the conclusion of the operation. Do not
use organic solvents for this purpose. Thoroughly clean protective garments at the conclusion of the operation and
store for reuse. Remove clothing which becomes contaminated as soon as possible and thoroughly clean before
reuse. Seek prompt medical assistance should a rash, chemical burn, or other adverse effect be experienced which
may be related to working with NOC. Do not store or consume food and tobacco in areas where they could be
contaminated with NOC.
b. Eye contact with NOC could result in chemical burns. Wear chemical safety goggles for all operations
where eye contact with NOC could occur. Additionally, use a full-length face shield for any operation where
splashing of the material could occur. In the event of eye contact, personnel should flush their eyes thoroughly with
fresh water for not less than 15 minutes, then seek prompt medical attention. An eye wash system conforming to the
design requirements of the American National Standards Institute (ANSI) Z358.1 shall be in the immediate vicinity
of all operations. Eye wash systems shall provide not less than 15 minutes of water for emergency flushing.
c. Over exposure to mists or vapors from NOC may result in sneezing, coughing, respiratory system irritation,
and possibly chemical burns and subsequent edema in the upper airways. Based on off-gas testing at temperatures
up to 180 degrees Fahrenheit (°F), such a possibility is unlikely, considering the magnitude and frequency of use. In
the event any adverse health effects are experienced, cease operations involving NOC and consult the cognizant
medical department representative for additional guidance.
4.3.1.3 Disposal. Disposal of NOC shall be in accordance with local, state, and federal regulations. If
neutralizing NOC, dilute at least 4:1 with water before adding acid to prevent forming a precipitate.
4.3.1.4 Compatibility. Appendix A gives the compatibility of NOC with various materials. Where specific
information is lacking, perform compatibility testing as specified in A.3.1 of Appendix A. NOC used to clean
aluminum or anodized aluminum shall be diluted 50 percent with water as specified in 4.3.1.6.
4.3.1.5 Inspection prior to use. The following inspections shall be performed prior to using NOC.
a. A shake test as specified in 5.13.2.2 and a visual inspection as specified in 5.13.3.2 shall be performed.
NOC which fails either inspection due to the presence of oil shall be rejected and returned to the vendor. NOC
which fails the visual inspection due to the presence of particulate or fiber shall be either filtered with a 5
micrometer nominal or finer filter to remove the suspended particulate or fiber or rejected and returned to the
vendor.
b. Activities verifying cleanliness using the non-volatile residue (NVR) by filtration procedure of Appendix B
shall sample one container or drum of each NOC lot or batch to determine the background NVR. NOC from
different lots or batches may be sampled from storage tanks, such as flushing rigs, to determine the background
NVR. For NOC fresh from a container, drum, or tank which has not been used, the baseline NVR shall be no
greater than 10 milligrams per liter (mg/L). NOC with greater than 10 mg/L NVR shall be rejected and returned to
the vendor or filtered with a 5 micrometer or finer filter and verified less than 10 mg/L NVR prior to use.
c. Government purchases of NOC are origin inspected, origin accepted with a Certificate of Analysis for each
lot maintained by the Defense Logistics Agency. Vendors purchasing NOC should request a Certificate of Analysis
with each delivery. Any NOC returned to a vendor because of a quality deficiency shall be noted (see 6.3).
4.3.1.6 Dilution. NOC shall be diluted as follows:
a. Concentration: NOC can be diluted with water up to 50 percent. NOC shall be diluted 50 percent with
Grade A or B water when cleaning aluminum or anodized aluminum.
b. Water quality: The preferred quality of water is 5 micrometer nominal or finer filtered Grade A water. For
long term use in cleaning equipment, such as an ultrasonic cleaning tank, parts washer, or flushing rig, Grade B
water may be used with a 1 micrometer nominal or finer filter installed. For short term use, such as a few hours,
Grade B water may be used with no filter.
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c. Order for mixing: In order to yield a more stable solution which will extend the life of the cleaner, water
should be added to NOC rather than adding NOC to water.
4.3.1.7 Use of NOC in previously used equipment. For cleaning equipment previously used with other than
NOC, the following actions should be taken to minimize and evaluate for the possibility of the NOC reacting with
the residue left behind.
a. Fill the cleaning equipment with NOC diluted 25 to 50 percent with Grade B water.
b. Operate the cleaning equipment covered for 4 hours at 140 to 160 °F.
c. Visually inspect the NOC for foam and precipitate. Visually inspect the equipment for milky white
deposits. Some white deposits at the fluid-air boundary are acceptable.
d. If precipitate is visible in the NOC, the NOC foams, or milky white deposits are visible on the equipment in
areas continuously wetted with NOC, discard the NOC solution, remove the deposits as specified in 4.3.1.7(e), and
repeat the process.
e. Deposits can be removed by soaking in hot water, or soaking and scrubbing with commercial white vinegar
or a warm (up to 110 °F) 10 to 16 percent citric acid solution followed by a water rinse. A 10 to 16 percent citric
acid solution can be prepared by adding 12 to 20 ounces of powdered citric acid (CAS No. 77-92-9) to one gallon of
water.
4.3.1.8 Use for extended periods. Extended use of NOC should be in covered equipment to minimize
evaporation. NOC can be recycled using filtration, and continuously used or reused, provided the following
conditions are satisfied:
a. A shake test as specified in 5.13.2.2 reveals no excessive foam.
b. A visual inspection as specified in 5.13.3.2 reveals no particulate, fiber, or oil.
c. A hydrocarbon or NVR inspection as specified in 5.13.2 reveals less than 5 parts per million (ppm) above
baseline.
d. An alkalinity test as specified in 5.13.5 indicates a satisfactory result. As the alkalinity of NOC is depleted
in use, the volume of NOC required to obtain the blue end-point specified in 5.13.5 increases. When the alkalinity
test measures 35 to 40 milliliters (mL) of NOC, the NOC is at risk of developing an insoluble precipitate. The NOC
should either be replaced, or a portion of the low alkalinity NOC removed and replaced with fresh NOC to restore
alkalinity. If evaporation concentrates the NOC causing the alkalinity test to measure less than 10 mL of NOC, the
NOC should be diluted with water as specified in 4.3.1.6 to restore the alkalinity to a nominal measured range of 15
to 30 mL of NOC. Do not attempt to adjust the alkalinity of 50 to 100 percent concentrated NOC by adding acid; an
immediate gel or precipitate will develop. Alkalinity of NOC in use or stored in cleaning equipment should be
checked weekly until the alkalinity test measures about 30 mL of NOC. Then, more frequent analysis should be
performed to ensure an insoluble precipitate does not form.
4.3.1.9 Filtration. For long term use in cleaning equipment such as large ultrasonic tanks or parts washers, a
filter sized at about 1-micrometer nominal should be installed. For use in a flushing rig, a 5-micrometer nominal or
finer filter shall be installed, and it is recommended that a filter sized at about 1-micrometer nominal be installed. A
5-micrometer filter prevents introducing significant contamination back into the system. A 1-micrometer filter
allows recycling and extending the use of NOC. It is also recommended that for flushing applications, a strainer be
installed upstream of the filter to remove large debris that can prematurely clog the filter. Filters used for the first
time shall be checked for extractable organic material by recirculating with clean NOC at 140 to 160 °F for not less
than 1 hour and then verifying organic cleanliness as specified in 5.13.2. Checking for extractable organic material
of filters is not required for filters from the same vendor and of the same material that previously tested
satisfactorily. A suitable filter material is thermally bonded, pleated polypropylene containing no plasticizer or
adhesive. The major advantage of disposable polypropylene filter cartridges is ease of use. Cleaning stainless steel
reusable filters can be difficult and time consuming. The large soil holding capacity of disposable filter cartridges
can often balance the cost of using smaller soil holding capacity stainless steel filters requiring frequent cleaning.
Filter housings should be configured with a vent on the top of the housing to allow removing oil that has separated
from the NOC. Verify with the manufacturer that the temperature, pressure, and flow ratings of any filters are
adequate for the intended application. Disposal of used filters or separated oil shall be in accordance with local,
state, and federal regulations.
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4.3.1.10 Stowage. NOC should be stored in covered containers to minimize evaporative losses. Stowage of
heated NOC for several days should only be in corrosion resistant metal, Teflon, or Teflon lined glass containers.
Long term stowage of heated NOC in plastic (other than Teflon), rubber, or glass containers will result in cleaner
degradation. Unheated NOC may be stowed in plastic or plastic lined containers provided the container has been
checked for extractable organic material. This is accomplished by filling the container with NOC for not less than
10 days and verifying organic cleanliness as specified in 5.13.2. Checking for extractable organic material of
containers is not required for containers from the same vendor and of the same material that previously tested
satisfactorily. Experience indicates that NOC can be successfully stored in aged uncolored or clear high density
polyethylene (HDPE) or polypropylene plastic containers. NOC can also be stored in steel containers having an
unplasticized low density polyethylene (LDPE) liner which is not adhesively bonded to the steel container similar to
A-A-58020. Stowage of NOC in colored plastic containers may contaminate the cleaner and adversely affect the
NVR analysis results. NOC allowed to dry on glass will result in a hard insoluble residue. Wide mouth glass
sample bottles with external safety coatings and Teflon lined caps are acceptable, as are sampling containers
manufactured from Teflon, Teflon lined glass, Teflon lined plastic, or stainless steel. Bulk shipboard stowage of
NOC shall be in accordance with NAVSEA S9086-WK-STM-010/CH-670 for alkalies.
4.3.2 Tribasic sodium phosphate (TSP).
4.3.2.1 Applicability. TSP is a solid crystalline material mixed with water to prepare an aqueous alkaline
cleaning solution approved for use as a pre-cleaner or final cleaner for all compatible piping and components other
than liquid oxygen generating plants. It may be used for liquid oxygen generating plant piping and components
provided the aqueous cleaning process specified herein can be successfully accomplished. TSP shall be in
accordance with O-S-642, Type I or II, or equal. Type II is recommended because it is less susceptible to
precipitation.
4.3.2.2 Safety precautions. Follow the safety precautions recommended in the vendor’s material safety data
sheet and the following:
a. TSP is a solid, crystalline material which has a caustic action on skin, eyes, and mucous membranes.
Repeated or prolonged contact with the solid material or its solution shall be avoided.
b. Skin contact with TSP will result in irritation of the skin, including redness and burning of the skin, and
other skin damage. Wear impervious protection clothing (gloves, aprons or coveralls, boots) constructed of
neoprene or other material of equivalent resistance to penetration so as to prevent skin contact. If skin contact
occurs, exposed areas shall be washed with large amounts of fresh water. Remove clothing which becomes
contaminated as soon as possible and launder before reuse. If skin is damaged, seek immediate medical attention. If
skin is not damaged and symptoms persist, seek medical attention. If irritating dust or solution mist is present,
approved respirators shall be worn to avoid inhalation.
c. Eye contact with TSP could result in permanent eye injury, including injury of the cornea causing
blindness. Symptoms include stinging, tearing, redness, and swelling of eyes. Wear chemical safety goggles for all
operations where eye contact with TSP could occur. Additionally, use a full-length face shield for any operation
where splashing of the material could occur. In the event of eye contact, personnel should flush their eyes
thoroughly with fresh water for not less than 15 minutes, then seek prompt medical attention. An eye wash system
conforming to the design requirements of the ANSI Z358.1 shall be in the immediate vicinity of all operations. Eye
wash systems shall provide not less than 15 minutes of water for emergency flushing.
d. In the event any adverse health effects are experienced, cease operations involving TSP and consult the
cognizant medical department representative for additional guidance.
4.3.2.3 Disposal. Disposal of TSP shall be in accordance with local, state, and federal regulations.
4.3.2.4 Compatibility. Appendix A gives the compatibility of TSP with various materials. Where specific
information is lacking, perform compatibility testing as specified in A.3.1 of Appendix A.
4.3.2.5 Solution preparation. Prepare the TSP cleaning solution by dissolving 2 pounds of Type I or 4.5 pounds
of Type II TSP with 5 gallons of Grade B water at 160 to 180 °F. In order to prevent a violent reaction and to more
completely mix the TSP, add the TSP to the water; do not add water to the TSP. The solution shall be circulated
until the TSP is dissolved prior to exposing the solution to a system or component.
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4.3.2.6 Stowage. If a TSP stowage tank is not large enough, do not mix a solution stronger than as specified in
4.3.2.5 and attempt to dilute it in the piping system. Failure to maintain the temperature of a solution stronger than
as specified in 4.3.2.5 at 160 to 180 °F can result in the TSP precipitating and developing a harden mass. This
hardened mass is difficult, if not impossible, to remove. The preferred stowage tank material is stainless steel. Bulk
shipboard stowage of TSP shall be in accordance with NAVSEA S9086-WK-STM-010/CH-670 for alkalies.
4.3.3 Non-ionic detergent (NID).
4.3.3.1 Applicability. NID is a concentrated non-ionic hydrocarbon surfactant that is mixed with water, NOC,
or TSP solutions to prepare an aqueous detergent cleaning solution acceptable for use as a pre-cleaner. NID shall be
in accordance with MIL-D-16791, Type I, or commercial equivalent, such as Triton X-100.
4.3.3.2 Safety precautions. Follow the safety precautions recommended in the vendor’s material safety data
sheet (MSDS). In the event any adverse health effects are experienced, cease operations involving NID and consult
the cognizant medical department representative for additional guidance.
4.3.3.3 Disposal. Disposal of NID shall be in accordance with local, state, and federal regulations.
4.3.3.4 Compatibility. Appendix A gives the compatibility of NID solutions with various materials. The
compatibility of solutions of NID with NOC or TSP shall refer to the respective compatibility tables for NOC or
TSP specified in Appendix A. If necessary, perform compatibility testing as specified in A.3.1 of Appendix A.
4.3.3.5 Solution preparation. Prepare NID solution by adding 0.1 to 0.5 ounces of NID to each gallon of water.
Prepare NOC and NID solution by adding 0.1 to 0.5 ounces of NID to each gallon of NOC diluted 50 percent with
water. Prepare TSP and NID solutions by adding 0.1 to 0.5 ounces of NID to each gallon of water containing 8 to
12 ounces of TSP. NID solutions shall be used at temperatures not greater than 140 °F. At temperatures greater
than 140 °F, the solubility of NID will decrease leading to possible precipitation of NID.
4.4 Cleaning solvents.
4.4.1 NAVSEA approved halogenated solvents.
4.4.1.1 Applicability. A NAVSEA approved halogenated solvent, as specified in Appendix E, shall be used as
a final cleaner for instruments as specified in 5.4, for liquid oxygen generating plants and plant piping as specified in
5.8, and for field wipe as specified in 5.10.1.1 and 5.12.4. Use of a NAVSEA approved halogenated solvent for any
other application requires local engineering, environmental, and industrial hygiene approval.
4.4.1.2 Safety precautions. For any NAVSEA approved halogenated solvent, follow the safety precautions
recommended in the vendor’s material safety data sheet and the following:
a. At least two people shall be present at all times while solvent is being used. Do not leave the area
unattended while cleaning is in progress.
b. When a halogenated solvent is being transferred by hose or pipe from a remote location, communication
shall be established between the pumping station and the space involved.
c. To permit escape in the event of an accidental spill, a self-contained breathing device shall be immediately
available to each person in any space where operations involving a halogenated solvent are taking place or occupied
spaces where leaks may occur while systems containing halogenated solvents are being cleaned, tested, serviced, or
repaired. Each person shall have received instruction and practice in the use of the particular self-contained
breathing device to be used. When a spill occurs, a high concentration of solvent vapor may rapidly fill the space
and dilute the air in the space. Breathing this diluted, contaminated air can result in rapid (10 to 15 seconds) loss of
consciousness caused by oxygen being washed from the lungs. It is therefore necessary to stop breathing until the
self-contained breathing device has been put on and is supplying air. The Navy “Emergency Escape Breathing
Device” (EEBD) may be used for emergency escape.
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d. All hot work in the space shall be suspended before introducing the solvent into the system. An exception
is that during overhaul in a shipyard, hot work may be performed on board a ship while systems are being flushed
(not pressure tested) with halogenated solvents if each operation is authorized by a gas free engineer. Personnel
shall be instructed to leave the area immediately if anyone experiences any irritation of the eyes, nose, or throat.
During specially authorized hot work, self-contained breathing devices for emergency escape are not required in
spaces where all lines being flushed contain only welded joints (no flanges, valves, or other fittings having
mechanical joints). The following caution sign shall also be displayed at the entrance to all work spaces:
WARNING
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m. Halogenated solvents used in contact with Diver Life Support Systems shall be completely drained and
placed in an oven or heated to ensure all solvent is volatilized and removed before assembly, test, and operation. Air
samples as specified in 5.9.3 are required to confirm removal of all solvent.
4.4.1.3 Disposal. Disposal of NAVSEA approved halogenated solvents shall be in accordance with local, state,
and federal regulations. Used or contaminated halogenated solvent should be reclaimed for use by distillation or
other appropriate method and inspected as specified in applicable specifications (see 6.3).
4.4.1.4 Compatibility. Appendix E gives the compatibility of NAVSEA approved halogenated solvents with
various non-metallic materials. Where specific information with respect to compatibility is lacking, perform
compatibility testing as specified in A.3.1 of Appendix A.
4.4.1.5 Use of NAVSEA approved halogenated solvents. Follow the instructions provided by the vendor and
as directed herein.
4.4.1.6 Water previously used in systems. Many halogenated solvents will react with water forming corrosive
acids. Systems previously known or believed to contain water or aqueous cleaning solutions shall be purged with
nitrogen as specified in 4.7.3. An outlet dew point of minus 40 °F shall be obtained prior to introducing a
halogenated solvent.
4.4.2 Isopropyl alcohol.
4.4.2.1 Applicability. Isopropyl alcohol (IPA) is an approved cleaning solvent for use only as a pre-cleaner for
compatible materials. IPA shall not be used as a pre-cleaner for Teflon which will be wetted by an oxygen-enriched
fluid. IPA should be in accordance with TT-I-735 or equal. IPA is soluble in water and commercial grades can have
as much as 30 percent water.
4.4.2.2 Safety precautions. Follow the safety precautions recommended in the vendor’s material safety data
sheet and the following:
a. IPA is a volatile hydrocarbon solvent with a boiling point of about 180 °F. IPA is extremely flammable
having a flash point of 56 °F. IPA vapors are toxic having a recommended 8-hour time weighted average exposure
criteria of 400 ppm. Ingestion of IPA will cause burning of the gastrointestinal tract, nausea, vomiting, bleeding,
central nervous system (CNS) depression, hemolysis, and pulmonary damage. Ingestion of as little as 10 mL may
cause serious injury, while ingestion of 240 mL can be fatal.
b. An industrial hygienist, gas-free engineer, gas-free person, or other designated individual shall verify that
ventilation in the space is adequate to keep the concentration of the solvent below the recommended exposure
criteria during anticipated operations, excluding accidents or spills. Use caution when ventilating IPA vapors since
the vapors are flammable. Explosion-proof equipment may be necessary.
c. IPA is absorbed by non-metallic material, such as Teflon, and unless carefully dried may off-gas flammable
and toxic material. Commercial grades of IPA, including TT-I-735, will leave a residue that may be flammable in
an oxygen enriched atmosphere.
d. In the event any adverse health effects are experienced, cease operations involving IPA and consult the
cognizant medical department representative for additional guidance.
4.4.2.3 Disposal. Disposal of isopropyl alcohol shall be in accordance with local, state, and federal regulations.
4.4.2.4 Compatibility. Where specific information with respect to compatibility is lacking, perform
compatibility testing as specified in A.3.1 of Appendix A.
4.5 Other cleaners.
4.5.1 Other pre-cleaners. Any compatible aqueous cleaning solution or cleaning solvent may be used as a pre-
cleaner with local engineering and environmental approval. Directions for use, safety precautions, disposal, and
compatibility are the responsibility of the approving activity. For all Naval activities, review by the cognizant
medical department or industrial hygienist shall be obtained prior to locally approving the use of any aqueous
cleaning solution or cleaning solvent other than those specified in 4.3 or 4.4.
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4.5.2 Other final cleaners. No aqueous cleaning solutions other than TSP solutions, or MIL-DTL-24800
compositions shall be used as a final cleaner. Other than the NAVSEA approved halogenated solvents, approval
shall be obtained prior to using any other cleaning solvent as a final cleaner (see 6.3). Activities interested in
obtaining approval of other final cleaning solvents or processes shall obtain direction (see 6.3).
4.7.2 Helium. Helium shall be the preferred test gas for helium and helium-oxygen components and systems
when performing tightness tests. Helium or nitrogen are the preferred purge gases for all applications. Helium shall
be in accordance with MIL-PRF-27407, Type I, Grade B. Helium shall be filtered to 10 micrometers nominal or
less. Helium may be used in place of nitrogen for tightness testing with local engineering approval. However, note
that helium may leak past mechanical joints or seats so that systems that are tight with nitrogen may demonstrate
leakage when tested with helium. If residual helium in a system will present a problem, it shall be purged with the
appropriate gas as required.
4.7.3 Nitrogen. Nitrogen shall be the preferred drying gas for all applications and test gas for hydrogen,
oxygen, and nitrogen systems and components when performing tightness tests. Nitrogen or helium are the
preferred purge gases for all applications. Nitrogen shall meet, by vendor or laboratory statement of conformance,
the requirements of A-A-59155, Grade A or B, or MIL-PRF-27401, Type I, Grade B or C, or CGA G-10.1, Grade L
or M. Nitrogen shall be filtered to 10 micrometers nominal or less. If residual nitrogen in a system will present a
problem, it shall be purged with the appropriate gas as required.
4.7.4 Oxygen. Oxygen shall only be used in a system or component specifically designed and cleaned for
oxygen service. When effected joints can be continuously monitored for leakage, oxygen may be used for tightness
testing with local engineering approval. No other use of oxygen for tightness testing shall be permitted.
4.7.5 Argon. When argon is specified to support welding, it is an acceptable purge gas. Argon shall meet, by
vendor or laboratory statement of conformance, the requirements of MIL-PRF-27415, Type I, Grade A. Argon shall
be filtered to 10 micrometers nominal or less. If residual argon in a system will present a problem, it shall be purged
with the appropriate gas as required.
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4.8 Cleaning silver-brazed piping. For systems with new silver-brazed joints, residual silver-brazing flux shall
be prevented or removed by one of the following procedures:
a. Systems cleaned with a NAVSEA approved halogenated solvent can either be brazed using the low flux
procedure in accordance with NAVSEA S9086-CH-STM-010/CH-074, Volume 1, or the joint can be locally cleaned
to remove the brazing flux. Halogenated solvents are not effective in removing brazing flux and systems cleaned
with halogenated solvents can not be soaked or flushed with water to remove residual flux due to difficulties in
drying the system.
b. For systems that will be cleaned with a NOC or TSP aqueous oxygen cleaning process, residual brazing
flux can be removed in accordance with NAVSEA 0900-LP-001-7000 prior to cleaning, or residual brazing flux can
be removed with the aqueous oxygen cleaning process. In either case, the brazing flux shall be removed prior to the
hydrostatic test. When using an aqueous oxygen cleaning process to remove brazing flux from copper tubing, NOC
is preferred because it does not discolor copper like TSP.
c. For systems that will be cleaned with water such as the boundary defined by 1.2.2.4, remove residual
brazing flux in accordance with NAVSEA 0900-LP-001-7000, and then clean as specified herein.
4.9 Lubricants. Lubricants shall be oxygen compatible in accordance with NAVSEA S9086-H7-STM-010/CH-
262 (see 6.3). During reassembly, lubricants shall be used sparingly. Direct contact of a lubricant with an oxygen or
oxygen enriched atmosphere should be avoided. Excessive quantities of lubricant can trap particulate and other
contaminants developing a potential fire hazard. Avoid the use of fluorinated lubricants with aluminum and
magnesium under conditions of large shear such as threaded connections. Ignition of fluorinated lubricants has
occurred in these applications.
5. DETAILED REQUIREMENTS
5.1 Facility requirements. Unless otherwise specified, the cleaning of components and assembling, testing, and
packaging of components cleaned as specified in this standard shall be performed in a cleanroom. A general
exception is nitrogen-oxygen life support components wetted by not greater than 50 percent by volume oxygen and
demineralized water system components which can be cleaned, assembled, tested, and packaged in a controlled area.
Other operations, including removal, replacement, and repair of piping and components cleaned as specified in this
standard, shall be performed in either a cleanroom or controlled area unless otherwise specified in Table IX.
Cleanroom and controlled area requirements shall be as specified in Table II and 5.1.1 through 5.1.7.
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5.1.1 Structure.
5.1.1.1 Class A. Class B requirements shall apply. Additionally, best commercial practices shall be employed
in the use of materials, construction, filtration, clothing, personnel, and temperature, pressure, and humidity control
to achieve an airborne particulate cleanliness level equivalent to ISO 14644-1 and 14644-2, Class 8, or better. Refer
to MIL-HDBK-407 for additional guidance.
5.1.1.2 Class B.
a. A permanent enclosure comprised of a rigid frame with clearly defined walls, ceilings, and floor, all
adequate to prevent the entry of contamination from the surrounding environment.
b. The surface of the walls, ceiling, and floor shall be fabricated or coated with material that minimizes
attraction of dirt and is easily cleaned. Refer to MIL-HDBK-407 for additional guidance.
c. Where dirt may be brought into the clean area, preventative measures such as anterooms, shoe covers, or
tack mats shall be employed. Anterooms should provide for changing and stowing of clothing, examination of tools
and equipment, and personnel access to the clean area. Washing, toilet facilities, and storage facilities for
maintenance of equipment should be provided in the immediate area where desirable.
d. Furnishings and equipment such as work benches, chairs, and racks shall be constructed and finished with
materials that will not produce dust or particulate as a result of chipping, flaking, or rusting. Paint should be hard
and non-flaking or non-chalking. Furnishings likely to be abraded or bumped should be constructed of either
stainless steel or non-fracture type plastic. Refer to MIL-HDBK-407 for additional guidance.
e. Work that produces airborne dust, dirt, or particulate should not be performed in a cleanroom. Welding and
brazing shall not be performed in a cleanroom.
5.1.1.3 Class C. Air borne debris or contamination resulting from work accomplished in the controlled area
shall be eliminated before redesignation as a controlled area. Depending on the time and work involved for a
particular operation, a controlled area shall be one of the following:
a. Clean space located or set up adjacent to areas which are non-contaminant producing.
b. Clean tent or partitioned and covered area. The clean-tent shall be established by taping clean, unused,
polyethylene plastic sheets in accordance with MIL-PRF-22191, Type I, or equal, on the deck, overhead, and
vertical areas for a distance of 3 to 4 feet around the area concerned. The outside surfaces of exposed materials
within the confined area shall be cleaned to remove dust, oil, dirt, and other foreign material. Air movement within
the confined area shall be held to minimum.
c. Clean glove box or isolation box with a clean atmosphere. The glove box is a temporary enclosure
surrounding the work area and sealed from the outside atmosphere. Work is accomplished through plastic gloves
sealed to the box walls.
d. A sleeve, with a clean, dry, nitrogen supply or equally clean, dry, air supply.
5.1.2 Maintenance.
5.1.2.1 Class A. Class B requirements shall apply. Additionally, when specified, a particle count of the
laminar flow benches and each clean area should be accomplished daily.
5.1.2.2 Class B.
a. Complete cleaning and wipe-down of equipment, tools, workbenches, counters, table tops, and fixtures
with detergent such as NID specified in 4.3.3, or commercial equivalent, and vacuuming and mopping of the floor
shall be accomplished at the end of each 8 hours of operation and prior to use if greater than 24-hours has passed
since the cleanroom was last used.
b. Complete cleaning and wipe-down of the walls, floors, and ceiling with detergent such as NID specified in
4.3.3, or commercial equivalent, shall be accomplished monthly.
c. The average air temperature and average humidity in a cleanroom shall be measured daily.
d. Air filters shall be cleaned or replaced at regular intervals.
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e. Oil, grease, residue, spilled chemicals, and any foreign material which develop in the area shall be cleaned
immediately. Chips, particles, and dust generated during any operation shall be removed during the operation by
vacuum.
f. No eating, drinking, smoking, or personnel grooming is allowed. Drinking fountains are permissible.
g. Only oxygen approved lubricants as specified in 4.9 shall be stored and used. Items incompatible with
oxygen such as hydrocarbon oil and grease and wood shall not be stored or used.
5.1.2.3 Class C.
a. Complete cleaning and wipe-down of equipment, tools, work surfaces, and fixtures with detergent such as
NID specified in 4.3.3, or commercial equivalent, and vacuuming and mopping of the floor, if applicable, shall be
accomplished at the end of each 8 hours of operation and prior to use if greater than 24 hours has passed since the
controlled area was established.
b. Air filters, if installed, shall be cleaned or replaced at regular intervals.
c. Oil, grease, residue, spilled chemicals, and any foreign material which develop in the controlled area shall
be cleaned immediately. Chips, particles, and dust generated during any operation shall be removed during the
operation by vacuum.
d. No eating, drinking, smoking, or personnel grooming is allowed. Drinking fountains are permissible.
e. Only oxygen approved lubricants as specified in 4.9 shall be stored and used. Items incompatible with
oxygen such as hydrocarbon oil and grease and wood shall not be stored or used.
5.1.3 Temperature and humidity. The temperature and humidity ranges indicated are recommendations only.
Exceeding the recommended ranges may result in personnel discomfort, build-up of static charges if the humidity
drops below 30 percent, or rusting of equipment and the enclosure if the humidity exceeds 50 percent. More
stringent requirements may apply if other work, such as calibration, is being performed.
5.1.4 Air filtration.
5.1.4.1 Type A. The best commercial practice employing items such as high efficiency particulate air (HEPA)
filters shall be used to achieve and maintain the airborne particulate cleanliness level as specified in Table II,
footnote 1/.
5.1.4.2 Type B. Outside and recirculated air shall be filtered to remove dust particles. Filter nominal rating
shall be less than 10 micrometers.
5.1.5 Ventilation and air pressure.
5.1.5.1 Class A. The cleanest room should have a positive pressure of not less than 0.05 inches of water above
the ambient pressure. A differential pressure of not less than 0.01 inches of water should exist between any
enclosure within the cleanroom and any adjacent area of lesser clean requirements.
5.1.5.2 Class B. The ventilation air supply shall maintain a slight positive pressure so that the air flow will
always be outward from the clean area.
5.1.5.3 Class C. Ventilation shall be employed as necessary to prevent the entry of contaminants from
surrounding areas and to keep the concentration of any solvent in use not greater than its recommended exposure
criteria. Fully contained uninhabited areas such as glove bags shall employ ventilation as necessary to prevent the
introduction of contaminants.
5.1.6 Personnel clothing.
5.1.6.1 Class A. Strict control of personnel and their clothing is required to achieve and maintain a critical
cleanroom. At a minimum, Class B requirements shall apply. Additional items such as full coveralls with hoods
and booties, anti-static gloves, lint-free paper, and limitations on personnel with skin ailments and colds are
generally employed. Refer to MIL-HDBK-407 for guidance in establishing the requisite additional personnel and
clothing requirements.
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5.1.6.2 Class B.
a. Clean undamaged coveralls or smocks, without buttons, exposed zippers, keys, and similar articles shall be
worn by all personnel including visitors and observers. Clothing should not be worn open or worn outside of the
cleanroom or controlled area.
b. Where dirt could be brought in from the outside, shoe covers shall be worn.
c. Clean items shall only be handled with clean gloves such as latex, vinyl, or polyethylene which are free of
lint and powder. Gloves in contact with cleaning solvents or solutions shall be chemically resistant for personnel
safety and to prevent spread of contamination to oxygen clean surfaces. Oxygen clean surfaces touched with bare
hands shall be considered contaminated.
d. Special precautions shall be taken in the case of opened piping and components to prevent the introduction
of loose articles such as buttons, jewelry, pens, coins, glasses, contact lenses, and hearing aids. Badges, where
required to be worn, shall be securely fastened to the clothing.
5.1.6.3 Class C.
a. Clean undamaged clothing with firmly affixed buttons and zippers shall be worn by all personnel including
visitors and observers.
b. Tack mats or shoe covers shall be used if dirt could be brought in from the surrounding area.
c. Clean items shall only be handled with clean gloves such as latex, vinyl, or polyethylene which are free of
lint and powder. Gloves in contact with cleaning solvents or solutions shall be chemically resistant for personnel
safety and to prevent the spread of contamination to oxygen clean surfaces. Oxygen clean surfaces touched with
bare hands shall be considered contaminated.
d. Special precautions shall be taken in the case of opened piping and components to prevent the introduction
of loose articles such as buttons, jewelry, pens, coins, glasses, contact lenses, and hearing aids. Badges, where
required to be worn, shall be securely fastened to the clothing.
5.1.7 Tools and equipment. Tools and equipment brought into a cleanroom or controlled area shall be free of
visible soil and particulate. Tools and equipment used in direct contact with oxygen clean surfaces shall be cleaned
in accordance with this standard. Where the configuration of the tool or equipment prevents cleaning in accordance
with this standard such as micrometers and dial indicators, all exposed surfaces shall be wiped clean with an
approved final cleaning solvent or solution and inspected as specified in 5.13.1 for visual cleanliness.
5.2 Aqueous component cleaning process.
5.2.1 Applicability. This aqueous component cleaning process is applicable to items that can be fully immersed
in the ultrasonic tank or parts washer specified in 5.2.3. Large components such as flasks shall be cleaned as
specified in 5.3 (see 6.3).
5.2.2 Objective. The objective of the aqueous component cleaning process is to remove all visible soil and
particulate during the pre-clean and rinse step as specified in 5.2.4 before proceeding to a final clean, verification,
and rinse step as specified in 5.2.5. The objective of the final clean, verification, and rinse step is to apply an oxygen
and life support safe cleaning agent to remove thin soil films and particulate that may remain after the pre-clean step
and to verify the required cleanliness. An effective pre-clean step increases the probability of a successful final
clean and verification step reducing overall process cost and time.
5.2.3 Material and equipment.
a. A supply of rinse water and associated equipment such as sinks, spray nozzles, and ultrasonic tanks.
b. A supply of compatible pre-cleaner as specified in 4.3, 4.4, or 4.5 and associated equipment such as
brushes, sinks, spray nozzles, and ultrasonic tanks.
c. A supply of NOC or TSP final cleaner as specified in 4.3 in an ultrasonic tank or a parts washer as specified
in 5.2.3(f).
d. A supply of nitrogen if used for drying.
e. An oxygen clean facility as specified in 5.1.
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f. An ultrasonic cleaning tank of sufficient size to allow complete immersion of the component being cleaned.
The tank shall be heated to 160 °F for NOC or 180 °F for TSP. Tanks using NOC should have a recirculating pump
system and filter as specified in 4.3.1.9. The tank shall have a generator frequency of at least 25 kHz and a
generator power per radiated surface of at least 3 watts/in2. The power per radiated surface area can be determined
by dividing the total generator power by the surface area of tank bottom or side where the generator transducers are
located. For example, a tank of dimensions 12 inches by 12 inches by 11 inches deep with a 600 watt transducer
mounted on the bottom has a power of 4.2 watts/in2, or
A parts washer of sufficient size to completely contain the component being cleaned. The parts washer shall
completely immerse the component in the cleaning agent and shall direct cleaning agent across or through the
component at a fluid velocity of not less than 3 feet per second (ft/sec). The parts washer shall be heated to 160 °F
for NOC or 180 °F for TSP. Parts washers using NOC should have a recirculating pump and filter selected as
specified in 4.3.1.9.
g. Equipment to dry oxygen clean parts.
h. Equipment to perform the applicable analyses as specified in 5.13. This includes clean 1-liter containers as
specified in Appendix B or C to obtain the required samples.
i. Packaging material as specified in 5.16.
5.2.4 Pre-clean and rinse. Pre-cleaning should be accomplished in a well ventilated area outside of the
cleanroom as follows:
a. Each component shall be pre-cleaned using a compatible pre-cleaner and then rinsed with water until all
visible soil, particulate, and cleaning agent is removed. Components shall be disassembled to achieve maximum
cleanliness. Components which are visibly clean may eliminate the pre-clean step and proceed directly to the final
clean, verification, and rinse step as specified in 5.2.5.
b. Rinsing of corrosion resistant metals such as stainless steel, nickel-copper (monel), and copper-nickel may
use Grade C water provided temperatures are less than 140 °F. At higher temperatures, or where municipal water
supplies leave undesirable deposits, Grade B water shall be used.
c. When using multiple pre-cleaners, rinse between each different pre-cleaner application to prevent any
harmful reaction which may occur when different cleaning agents are combined.
d. When removing difficult soils such as heavy waterproof greases, silicone greases, and fluorinated greases,
most pre-cleaners will have limited effectiveness if used without agitation in a soak or ultrasonic tank. Hand
scrubbing is often the best alternative.
e. Components shall be dried if the delay between completion of pre-cleaning and start of final cleaning could
result in the formation of rust or other oxides. Otherwise, no specific drying step is required prior to final cleaning.
5.2.5 Final clean, verification, and rinse. Final cleaning, verification, and rinsing shall be accomplished as
follows:
a. Fully immerse components in an ultrasonic tank or parts washer filled with NOC at 140 to 160 °F or TSP at
160 to 180 °F.
b. Energize the ultrasonic tank or parts washer for 5 to 15 minutes. For components such as O-rings and valve
seats, limit exposure to a maximum of 10 minutes.
c. Obtain a 500 to 600 mL sample of the used NOC or TSP in a 1-liter container and verify organic
cleanliness as specified in 5.13.2. If any analysis fails, replace the final cleaner and repeat the final clean,
verification, and rinse process. Do not wait for the results of 5.13.2 before proceeding to rinsing as specified in
5.2.5(d). When cleaning large quantities of parts on a regular basis or when cleaning with an automated process,
statistical process control can be implemented (see 6.3). Statistical process control could entail, for instance,
sampling every fourth batch. If the fourth batch fails, the previous three batches also fail and require recleaning.
d. Remove the component(s) from the ultrasonic tank or parts washer and immediately rinse with Grade B
water in an ultrasonic tank, batch tank, or flowing water. The rinse water shall be not less than 110 °F for NOC and
120 °F for TSP. Continue rinsing until the effluent rinse water pH measured as specified in 5.13.4.2 is 8.0 or less,
but rinse for not less than 30 seconds. The preferred rinse process consists of two rinses using an ultrasonic or batch
tank as the first rinse followed by a batch tank or flowing water as the second rinse.
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e. Obtain a sample of not less than 200 mL of the effluent rinse water and verify particulate cleanliness as
specified in 5.13.3. If the particulate analysis of 5.13.3 fails, replace the rinse water if applicable and repeat the final
rinse step.
5.2.6 Dry, reassemble, and package. Drying, reassembling, and packaging shall be accomplished in an oxygen
clean facility as follows:
a. Components shall be dried until no moisture is visible using any method that does not result in loss of
cleanliness. Ovens, vacuum ovens, dryers, heat guns, and dry filtered nitrogen have been successfully used. The
method chosen for drying shall be verified oxygen clean during the validation process as specified in 5.15.
Appropriate precautions shall be taken to prevent damaging components, gaskets, and seals from excessive heat.
For components with inaccessible areas, drying to plus 20 °F dew point is acceptable.
b. During reassembly, use oxygen compatible lubricants as specified in 4.9 sparingly.
c. Components shall be packaged as specified in 5.16.
5.3 Flask cleaning and inspection.
5.3.1 Applicability. Flask cleaning and inspection is applicable to flasks in the boundaries defined in 1.2.
5.3.2 Material and equipment.
a. A supply of rinse water and associated equipment for rinsing flasks.
b. A supply of NOC or TSP final cleaner as specified in 4.3.
c. A supply of helium or nitrogen.
d. Equipment as required to perform visual inspection and clean the flask.
e. Equipment to perform the applicable analyses as specified in 5.13. This includes clean 1-liter containers to
obtain the required samples.
f. Equipment as required to remove paint from flask surfaces.
g. A dew point indicator equal to the Ondyne Series 1400 Dewpoint Indicator or the MCM Dewluxe Model
hygrometer capable of detecting a dew point of minus 40 °F (128 ppm H2O).
5.3.3 Clean, verification, and rinse. Cleaning, verification, and rinsing should be accomplished in a controlled
area with the flasks positioned vertically to facilitate drainage as follows:
a. Flasks final cleaned with a fill and recirculate process as specified in 5.3.3.(b) or 5.3.3.(c) shall be pre-
cleaned as specified in 5.2.4 using a compatible pre-cleaner and then rinsed with water until all visible oil, grease,
ink, dye, and cleaning agent is removed. Flasks final cleaned with a spray process as specified in 5.3.3.(b) or
5.3.3.(c), or flasks with no visual evidence of oil, grease, ink, or dye may eliminate the pre-clean step and proceed
directly to final clean.
b. If final cleaning flask interior surfaces with NOC, apply NOC at not less than 120 °F for a time sufficient to
ensure all wetted surfaces are in contact with the cleaner for not less than 10 minutes if using a spray process or at
150 to 170 °F for not less than 30 minutes if using a fill and recirculate process. Use of sprayers with high flow and
low pressure or low flow and high pressure are recommended.
c. If final cleaning flask interior surfaces with TSP, apply TSP at 160 to 180 °F for a time sufficient to ensure
all wetted surfaces are in contact with the cleaner for not less than 10 minutes if using a spray process or not less
than 30 minutes if using a fill and recirculate process. Use of sprayers with high flow and low pressure or low flow
and high pressure are recommended. When using TSP, the flask shall be preheated by circulating hot Grade B water
through the flask. In order to prevent precipitation of TSP, the TSP shall not be allowed to cool or remain
uncirculated prior to rinsing as specified in 5.3.3(e).
d. Obtain a 500 to 600 mL sample of the used NOC or TSP in a 1-liter container and verify organic
cleanliness as specified in 5.13.2. If any analysis fails, replace the cleaner and repeat the clean, verification, and
rinse process. Do not wait for the results of 5.13.2 before proceeding to rinsing as specified in 5.3.3(e).
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e. After flushing with NOC or TSP, immediately rinse the flask with Grade B water. For corrosion resistant
flasks, Grade C water may be used followed by a Grade B water rinse. The water temperature shall be adequate to
remove the cleaning agent. Continue rinsing until the effluent rinse water pH measured as specified in 5.13.4.2 is
not greater than 8.0. Do not dry the flask between cleaning and rinsing.
f. Recirculate or spray Grade B water through the flask for not less than 5 minutes. The water temperature
does not need to be elevated. Obtain a sample of the rinse effluent and verify particulate cleanliness as specified in
5.13.3. If the particulate analysis of 5.13.3 fails, repeat the rinse step.
5.3.4 Drying. Drying after exposure of a flask to water or moist gas, such as ambient air, shall be accomplished
as follows:
a. Dry the flask as quickly as possible with nitrogen until a minus 20 °F dew point is reached. Nitrogen
preheaters, strip heaters, or vacuum pumps have been successfully used. Appropriate precautions shall be taken to
prevent damaging the flask or support piping and equipment from excessive heat.
b. While maintaining cleanliness as specified in 5.10, perform a visual inspection on the internal flask surfaces
as specified in 5.13.1.2 and 5.13.1.3. Flask surfaces with evidence of oil, grease, ink, dye, particulate, or fibers shall
be recleaned. Flask surfaces with evidence of corrosion shall be blasted or tumbled as specified in 5.3.5.3.
c. While maintaining cleanliness as specified in 5.10, install end fittings and seal weld, if required, in
accordance with the applicable specification. Steel flasks shall be evacuated to 20 inches or less of mercury or
purged with nitrogen to remove moist air, and then pressurized to 5 to 15 lb/in2 with nitrogen.
5.3.5 In-service interior inspection. When interior inspections of in-service flasks are required for
recertification, the interior surfaces shall be inspected for evidence of corrosion, loose scale, particulate, grit, filings,
paint, oil, and grease as specified in 5.13.1.2 and 5.13.1.3. Interior surfaces shall also be inspected and the outside
surface of the flask marked to indicate the location of pits, cuts, burns, defects, and so forth. Pits, gouges, burns, arc
strikes, and other surface defects shall be treated in accordance with NAVSEA S9086-SY-STM-010/CH-551, CGA
C-6.1, or CGA C-6.2. Steel flasks shall be evacuated to 20 inches or less of mercury or purged with nitrogen to
remove moist air, and then pressurized to 5 to 15 lb/in2 with nitrogen immediately after the internal inspection if
satisfactory, or corrective action of 5.3.5.1 to 5.3.5.4 if unsatisfactory. Based on the interior inspection, flasks shall
be classified in accordance with the following criteria:
a. Satisfactory: Not more than 10 percent of the internal surface has evidence of corrosion or particulate, and
no evidence of loose scale, filings, paint, oil, or grease on the internal surface.
b. Unsatisfactory: More than 10 percent of the internal surface has evidence of corrosion or particulate, or
any evidence of loose scale, filings, paint, oil, or grease on the internal surface.
5.3.5.1 Flasks classified as unsatisfactory because of oil and grease shall be cleaned as specified in 5.3.3.
5.3.5.2 Flasks classified as unsatisfactory because of particulate or grit shall be flushed as specified in 5.3.3(f)
or vacuumed until a satisfactory interior surface as specified in 5.3.5(a) is obtained.
5.3.5.3 Steel flask surfaces classified as unsatisfactory because of corrosion and loose scale shall either be
blasted in accordance with MIL-F-22606 or tumbled in accordance with CGA C-6.1 and then flushed as specified in
5.3.3(f) or vacuumed to remove particulate until a satisfactory interior surface as specified in 5.3.5(a) is obtained.
Aluminum flask surfaces classified as unsatisfactory because of corrosion and loose scale shall be tumbled in
accordance with CGA C-6.1 and then flushed as specified in 5.3.3(f) or vacuumed to remove particulate until a
satisfactory interior surface as specified in 5.3.5(a) is obtained.
5.3.5.4 Flasks classified as unsatisfactory because of internal paint shall be blasted or chemically cleaned until a
satisfactory interior surface as specified in 5.3.5(a) is obtained. Flasks that have had interior paint removed by
chemical methods shall be off-gas tested as specified in 5.9.3 to ensure removal of all chemical. Additionally, MIL-
F-22606 flasks with evidence of internal paint shall be examined to determine the intended service of the flask.
Flasks identified as Service A, which are intended for air systems, shall be replaced with Service B flasks which are
intended for oxygen service.
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5.4 Cleaning and calibration of instruments and gauges. The requirements for cleaning instruments and gauges,
including flowmeters and dead-end pressure switches and transducers, within the boundaries defined in 1.2 shall be
in accordance with NAVSEA ST700-F1-PRO-010 (see 6.3) using a NAVSEA approved halogenated solvent.
Instruments and gauges should be calibrated in place by a comparative calibration procedure in accordance with
NAVSEA 0987-LP-022-3010.
5.5 Aqueous system cleaning process.
5.5.1 Applicability. The aqueous system cleaning process is applicable to all compatible systems other than
liquid oxygen generating plants. It may be used for liquid oxygen generating plant piping provided the aqueous
system cleaning process can be successfully accomplished. Flushing of ships service demineralized water system
piping shall be as specified in 5.7.
5.5.2 Material and equipment.
a. A supply of NOC or TSP as specified in 4.3 in a flushing rig as specified in 5.5.2(d).
b. A supply of rinse water in a flushing rig as specified in 5.5.2(d).
c. A supply of nitrogen.
d. A flushing rig consisting of tanks, pumps, piping, measuring devices for pressure, temperature, and flow,
hoses, filters, and strainers. All items shall be compatible with the cleaner and attain the pressure, temperature, flow
rates, and filtering required by this standard. Non-metallic material, other than seats, seals, and Teflon, wetted by
the cleaning solution shall be verified free of extractable organic material as specified in 4.3.1.9.
e. Equipment to perform the applicable analyses as specified in 5.13. This includes clean 1-liter containers to
obtain the required samples.
f. A dew point indicator equal to the Ondyne Series 1400 Dewpoint Indicator or the MCM Dewluxe Model
hygrometer capable of detecting a dew point of minus 40 °F (128 ppm H2O).
5.5.3 System preparation.
5.5.3.1 If shipboard conditions prevent flushing or testing a system as a single unit, the system may be divided
into sections and flushed accordingly. System sections may be flushed as required to accommodate items such as
interference problems and ship’s schedule. Precautions shall be taken to ensure that portions of the system which
have been certified oxygen clean are not flushed with contaminated cleaning agent. Local engineering shall review
the flushing paths or line-ups to ensure the system has been flushed and sampled.
5.5.3.2 The following items shall be accomplished to prepare a system for flushing:
a. Repairs to the piping system shall be completed before flushing is started.
b. Valves, valve internals, pressure regulators, filter elements, or other mechanically jointed components that
will interfere with the flow of the cleaning agent should be removed and flush plugs, spools, jumpers, and blanks
shall be installed. Where jumpers are used, their inside diameter should be not less than the piping they are
bypassing. Seal welded regulators may be left in place if the high pressure chambers are disassembled and the
nozzles removed.
c. Items having incompatible material that can be damaged during flushing shall be removed.
d. Components such as instruments which are not free draining shall be removed or isolated if appropriately
configured. Cleanliness of certified oxygen clean instruments shall be maintained as specified in 5.10.
e. Flow restrictors, if installed in the supply nipple upstream of the oxygen regulators, shall also be removed.
f. Flushing rig, including temporary piping, components, and flush plugs required for system flushing, shall
be pressure tested and cleaned to remove loose scale, dust, grit, filings, oil, and grease.
5.5.3.3 All removed items shall be cleaned as specified in 5.2. Where it is necessary to flush with valve
cartridges installed, after the flush, each cartridge shall be removed and cleaned as specified in 5.2.
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5.5.3.4 Large in-line volumes that will not support minimum flushing velocities should be individually cleaned
and bypassed during the final flush if possible. The concern is that NOC and TSP final cleaners remove soil by
displacement. In areas of low flow, suspended oil can separate from NOC or TSP and collect. If the volume cannot
be bypassed, cannot be inspected and locally cleaned as specified in 5.12.4, and will collect separated oil perform
the following: isolate the volume into the smallest flushing loop possible, obtain local engineering approval (see
6.3) to pre-clean by flushing with a low foaming detergent pre-cleaner that will emulsify oil contamination, and then
perform the preflush as specified in 5.5.6 prior to the final NOC or TSP flush. The pre-cleaner is used to remove oil
and grease contamination, and then NOC or TSP is used to remove any pre-cleaner residue and certify cleanliness.
For volumes that cannot be bypassed, but can either be locally cleaned as specified in 5.12.4 or the configuration of
the volume will not collect separated oil during the final flush, such as an in-line vertically oriented flask, a separate
pre-clean flush is not required.
5.5.4 Electrolytic oxygen gas generators. For systems with electrolytic oxygen generators, perform a potassium
hydroxide (KOH) contamination inspection as specified in 5.6.
5.5.5 Leak-check. The flush boundary shall be leak-checked with nitrogen or Grade B water to the anticipated
flush pressure. This will eliminate the time consuming clean-up of spilled or leaked cleaner. Where an oxygen
clean system interfaces with a flush boundary, using nitrogen for the leak check is recommended. Any nitrogen
leakage into the oxygen clean system will not cause loss of cleanliness.
5.5.6 Preflush. For new systems or systems with extensive modifications, a preflush as follows is
recommended:
a. Perform a forward and backward preflush at a minimum of 3 ft/sec using Grade B water. The preflush
water temperature may be elevated to not greater than 180 °F. The higher temperatures will increase the
effectiveness of the preflush and preheat the system minimizing the pipe line cleaning time.
b. Outlets should be opened one at a time to help clean valve bodies and other probable pocketing areas. The
flush should continue until there is no visible evidence of debris.
5.5.7 Hydrostatic test. Hydrostatic testing as specified in 5.9 should normally be accomplished after the
preflush, if applicable, and before the final flush.
5.5.8 Final flush or pipe line cleaning. The final flush or pipe line cleaning shall be accomplished as follows:
a. Flush the system with NOC at 150 to 170 °F or TSP at 160 to 180 °F at the flow rate as specified in
5.5.8(b). The temperature of the NOC at the outlet of the system being cleaned shall be maintained at not less than
140 °F. If TSP is used, the system shall be preheated by flushing once-through with hot Grade B water until the
desired temperature is attained. In order to prevent precipitation of the TSP, the TSP shall not be allowed to cool or
remain uncirculated prior to rinsing as specified in 5.5.9. If NOC is used, it may be recirculated in the system cold
and heated in place. The flush starts when the outlet temperature reaches 140 °F.
b. The fluid velocity shall be not less than 3 ft/sec. The flow rate in gallons per minute (GPM) equivalent to 3
ft/sec can be determined by multiplying the square of the pipe or tube inside diameter in inches by 7.4, as follows:
GPM at 3 ft/sec = (ID-inches)2(7.4)
c. The requirements for a back flush and the flush durations for various applications are as specified in
5.5.8(a) and Table III.
d. At the completion of the flush, obtain a 500 to 600 mL sample of the flushing medium in a 1-liter container
from each outlet prior to the filter. Sampling prior to the back flush is required only if new cleaning agent will be
used for the back flush. If the same charge of cleaner is used for both directions of the flush, only sampling at the
end of the flush is required.
e. For NOC, visually inspect the sample for oil and particulate. If oil or particulate is present, continue
flushing until no oil or excessive (3 or more particles) particulate is present. Continued flushing will allow the filter
to remove the visible contaminants. If no oil or excessive particulate is present, verify organic cleanliness as
specified in 5.13.2.
f. For TSP, verify organic cleanliness as specified in 5.13.2.
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g. If any analysis fails, replace the cleaning solution and repeat the final system flush. Do not wait for the
results of 5.13.2 before proceeding to rinsing as specified in 5.5.9.
TABLE III. Applicability matrix for flush duration and back flush. 1/
Configuration Flush duration Back flush
System contains socket welds, Not less than 60 minutes Not less than an additional 60
fittings, or components with minutes
expansions or contractions
System contains only bends and Not less than 30 minutes Not required
elbows and no socket welds, fittings,
or components with expansions or
contractions
Any configuration with all sections Not less than 30 minutes Not less than an additional 30
of piping fabricated from pre- minutes
cleaned piping and components
NOTE:
1/
Regardless of the configuration, the back flush can be deleted if all of the following conditions are met:
(a) It is authorized by local engineering.
(b) All pipe sections have been pre-cleaned.
(c) All valve bodies, filter housings, and other large component housings shall have been cleaned to oxygen
cleanliness requirements.
(d) Prior to the flush, all cartridges, filter elements, regulators, and other components shall be removed and
flush plugs or bypass lines installed. After the flush, all cavities shall be visually inspected as specified in
5.13.1. Any evidence of contamination shall be removed by either local cleaning with NOC or TSP or
additional flushing. The results of the visual inspection shall be recorded.
(e) For oxygen enriched systems only, the system piping and components shall be fabricated from material that
will not propagate a flame at maximum operating pressure when determined in accordance ASTM G94.
For information, brass, bronze, copper, copper-nickel, nickel-aluminum-bronze, and nickel-copper (monel)
will not propagate a flame in an oxygen or oxygen enriched atmosphere at pressures up to 7500 lb/in2.
5.5.9 Rinsing and particulate flushing. Rinsing and particulate flushing shall be accomplished as follows:
a. Remove the majority of NOC with nitrogen and collect for future use, or proceed to 5.5.9(b). When using
nitrogen, do not allow NOC to dry before proceeding to 5.5.9(b).
b. Remove cleaning solution by rinsing the system once-through with Grade B water at a velocity of not less
than 3 ft/sec. Return filters that were used during the flush step should be removed, replaced, or bypassed prior to
rinsing to prevent contamination trapped by the filter from being introduced into the system. The water temperature
shall be not less than 110 °F for NOC and 160 °F for TSP. Systems flushed with large in-line volumes, such as
moisture separators, where the flushing velocity is less than 3 ft/sec shall be back flushed with rinse water to ensure
all cleaning agent is removed.
c. Obtain a sample of the rinse effluent and measure the pH as specified in 5.13.4.2. When the effluent pH is
not greater than 8.0, outlets shall be opened one at a time to help clean valve bodies and other probable pocketing
areas. The rinse water shall then be recirculated until the pH of the effluent at each branch, vent, or drain is not
greater than 8.0.
d. At the completion of rinsing, obtain a sample of the rinse effluent from each branch and verify particulate
cleanliness as specified in 5.13.3. If any of the samples do not pass the required inspection, recirculate Grade B
water through the system at a velocity of not less than 3 ft/sec for not less than 30 minutes. The water temperature
does not need to be elevated. Filters should be installed to trap particulate. Continue flushing until a sample of the
effluent from each branch passes the particulate cleanliness as specified in 5.13.3.
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e. Any residual NOC or TSP in the cavities should be removed prior to drying. Remove flush plugs and
inspect for residual NOC or TSP. Remove all visible traces of NOC or TSP by wearing cleanroom gloves and
wiping each cavity and flush plug with a clean lint- free cloth wetted with Grade B water at a temperature of 100 to
120 °F. The flush plugs should be reinstalled prior to drying with nitrogen.
5.5.10 Drying and reinstalling components. Drying and reinstallation of components shall be accomplished as
follows:
a. Remove rinse water and dry the system with nitrogen until a minus 40 °F dew point is reached. For
systems which operate at elevated humidity, such as electrolytic oxygen generator systems, or in the absence of an
elevated dryness requirement, a dew point of plus 20 °F is acceptable. Nitrogen preheaters, strip heaters, or vacuum
pumps have been successfully used. Appropriate precautions shall be taken to prevent damaging piping and
equipment.
b. The recommended drying method is using nitrogen at low flow rates. This allows the gas to evaporate the
moisture. Higher flow rates are suitable for removing visible moisture. If it is suspected that pockets of water exist
at low points in the system, a high-volume blow-down can be employed. The pressure should be not greater than
100 lb/in2 or maximum operating pressure, whichever is less.
c. While maintaining cleanliness as specified in 5.10, all items shall be removed which were installed in
5.5.3.2. A visual inspection of each cavity shall be performed as specified in 5.13.1. Additionally, where
applicable, open and visually inspect all large volumes as specified in 5.13.1. If the visual inspection fails, locally
clean as specified in 5.12.4. While maintaining cleanliness as specified in 5.10, components cleaned as specified in
5.2 shall be installed:
d. The system shall be reassembled and pressurized with nitrogen or helium to maintain not less than 10 lb/in2,
or packaged as specified in 5.16 to maintain cleanliness. If the pressure should drop below 10 lb/in2, the responsible
authority shall investigate the circumstances associated with the pressure drop to ensure that no contamination could
have entered the system which would require repeating the flush.
e. Test, charge with system fluid, and return to operational conditions.
5.6 Potassium hydroxide (KOH) inspection.
5.6.1 Applicability. This inspection applies only if the system has an electrolytic oxygen gas generator that
uses KOH. The oxygen system shall be visually inspected for KOH contamination at mechanical joints before the
system is flushed as specified in 5.5.5 through 5.5.9. KOH is a whitish solid that may occur as a scale on the inside
of pipes and components.
5.6.2 Inspection. The inspection for KOH contamination shall be accomplished as follows:
a. The oxygen generator union connection shall be considered the first mechanical joint downstream of the
moisture separator. The piping to the oxygen generator union connection shall be examined for KOH
contamination. If no KOH is found, no further inspection shall be required. If contamination is found, perform the
inspection as specified in 5.6.2(b).
b. If KOH is found in the oxygen generator union connection as identified in 5.6.2(a), downstream piping to
the isolation valves in the distribution header shall be visually inspected. If no KOH is found in this section, no
further inspection is required and the KOH shall be removed as specified in 5.6.3. If KOH is found in this section,
the remainder of the system shall be visually inspected as specified in 5.6.2(c).
c. If KOH is found in the distribution header as identified in 5.6.2(b), the remainder of the system shall be
visually inspected. The KOH shall be removed as specified in 5.6.3.
5.6.3 KOH removal. KOH shall be removed by flushing with Grade B water at a temperature of 120 to 140 °F.
Flush until the conductivity of the effluent is within 2 micromhos of the influent, or the pH measured as specified in
5.13.4.2 is 8.0 or less. Dry as specified in 5.5.10.
5.7 Flushing of ships service demineralized water piping systems.
5.7.1 Applicability. This process applies to ships service demineralized water piping systems as defined in
1.2.2.4.
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5.7.2 Material and equipment. The following material and equipment are required:
a. A supply of Grade A water.
b. A flushing rig for flushing piping systems as specified herein. It shall consist of pumps, piping, measuring
devices for pressure, temperature, and flow, and hoses. Items shall attain the pressure, temperature, and flow rates
required by this standard.
c. Equipment to perform the applicable analyses as specified in 5.13.
5.7.3 Flush. Flushing shall be accomplished as follows:
a. The demineralized water piping shall be flushed for 15 minutes with Grade A water at not less than 150 °F
to remove loose scale, rust, grit, filings, oil, grease, and other foreign substances. Lower temperatures may be used
to prevent damage to items such as PVC piping with local engineering approval.
b. A sample of the flush water shall be inspected for particulate cleanliness as specified in 5.13.3 and verified
free of visual turbidity, oil, sediment, and resin beads. Resin beads or fines within the demineralizer are acceptable.
If organic contamination is suspected, determine the level of contamination in accordance with ASTM D4839, EPA
Method 9060A, or equal. Organic levels should not exceed 1 ppm.
5.7.4 Visual inspection. Following the flush, the system shall be inspected as follows:
a. Drain the water from the system and perform a visual inspection as specified in 5.13.1 except inspect only
for visible traces of hydrocarbons. The inspection shall be performed at the oxygen generator union connection, of
accessible surfaces in the demineralized water storage tank, and of distillate supply piping running from the
evaporator to the ships service demineralizer.
b. If visible traces of hydrocarbons are found, the piping shall be cleaned as specified in 5.5.
5.8 Solvent system cleaning processes.
5.8.1 Applicability. The solvent system cleaning processes are given in Table IV.
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5.8.2.3 Cleaning method. The cleaning method consists basically of dividing the plant’s producer, storage, and
pump-vaporizer process piping into a number of separate piping circuits by using the equipment’s isolation valves
and temporary jumper hoses and pipe closures. Each piping circuit is leak-checked prior to filling with solvent.
Solvent is then circulated through each piping circuit to be cleaned. A fill-and-soak method may be used for large
vessels such as distillation columns and storage tanks. Consult NAVSEA, the vendor, or the ship’s planning yard if
necessary to identify previously used cleaning procedures or to develop a specific procedure for the make and model
of the oxygen-nitrogen plant to be cleaned.
5.8.2.4 Sample and removal of cleaning solvent from system. The oxygen-nitrogen plant shall be certified
oxygen clean and free of cleaning solvent as specified in 5.8.3.4(b) and 5.8.3.4 (c). The gas cross connect piping
shall be sampled for cleaning solvent content as specified in 5.8.3.4 (c).
5.8.3 Oxygen-nitrogen plant piping.
5.8.3.1 Material and equipment. The following material and equipment are required:
a. A supply of cleaning solvent as specified in 4.4.
b. A supply of nitrogen.
c. A vacuum pump pulling not less than 25 inches mercury (Hg) vacuum for removing the cleaning solvent.
The pump design shall preclude pump lubricant from being drawn into the system being cleaned in the event of a
pump failure or stoppage. The pump shall be compatible with the cleaning solvent.
d. Gauges, flowmeters, and thermometers as required which are compatible with the cleaning solvent.
e. Equipment to perform the applicable analyses as specified in 5.13.
5.8.3.2 Preliminary joint tightness test. A preliminary joint tightness test shall be performed on the system
before introducing the cleaning solvent into the system piping. The preliminary joint tightness test shall be
performed with nitrogen to a minimum of 75 lb/in2 or the maximum system operating pressure if lower. Accessible
mechanical joints, seal welds, and disturbed welded joints shall be tightness tested using the test duration and
acceptance criteria as specified in 5.9 and Table VI.
5.8.3.3 Hydrostatic test. Hydrostatic testing as specified in 5.9 and Table V should normally be accomplished
before the final flush.
5.8.3.4 Flush. Flushing shall be accomplished as follows:
a. The system piping shall be flushed at not less than 3 ft/sec with cleaning solvent for not less than 30
minutes. If the flushing circuit is through parallel paths, if necessary, the flow paths shall be isolated to ensure that
each path is flushed with full flow for not less than 5 minutes followed by a 30-minute flush of the entire system
without full flow required in each leg.
b. Obtain a sample of the cleaning solvent from all sampling locations and verify organic cleanliness as
specified in 5.13.2 and verify particulate cleanliness as specified in 5.13.3. If any of the analyses fail, replace or
reclaim the solvent and repeat the flush.
c. After acceptable samples are obtained, the cleaning solvent shall be removed by draining and then purging
with low pressure nitrogen. A vacuum pump may be used in the final stages of solvent removal. Heat (200 °F
maximum) may be applied to the external surfaces of the piping to facilitate removal of the cleaning solvent. The
nitrogen exhaust shall be checked for traces of the cleaning solvent with a halide leak detector or equal. Evacuating
and purging shall continue until no trace of the solvent is detectable.
d. The system shall be pressurized with nitrogen to a minimum of 75 lb/in2 or the maximum system operating
pressure if lower. Samples of nitrogen under pressure shall be taken after a period of not less than 1 hour and
analyzed for solvent content. Samples shall be analyzed by gas chromatography or equivalent methods. The solvent
content shall not exceed 10 ppm. If this limit is exceeded, the system shall be purged with nitrogen until acceptable
samples are obtained.
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5.8.3.5 Maintenance of pressure in system. The system shall be maintained with not less than 10 lb/in2, or the
maximum system operating pressure if lower, of nitrogen until the system is charged with oxygen or nitrogen. If the
pressure should drop below 10 lb/in2 before charging, the responsible authority shall investigate circumstances
associated with the pressure drop to ensure that no contamination could have entered the system which would
require repeating the flush.
5.9 Testing.
5.9.1 Pressure testing. Piping and components defined by the boundaries of 1.2 shall be pressure tested
(hydrostatic, joint tightness, seat tightness, and pressure drop) as specified in Tables V through VIII. Flexible hoses
shall be tested in accordance with NAVSEA S6430-AE-TED-010. When contractually invoked, or otherwise
specified by NAVSEA, the test requirements of NAVSEA SS800-AG-MAN-010/P-9290 or NAVSEA SS521-AA-
MAN-010, or other NAVSEA approved procedure shall take precedence over Tables V through VIII.
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5.9.2 Operational testing. Repairs, modification, or installation of new piping and components which affect the
operation of the system or components require operational testing prior to manned use. Open-ended piping requires
an operational test to prove unobstructed flow.
5.9.3 Gas sampling and analysis. For critical applications and Diver Life Support Systems, a gas sample is
required if work was accomplished that could introduce gaseous contaminants into a component or system such as
cleaning with a solvent. For components with large volumes, such as flasks, the sample may be taken prior to or
after installation, however, sampling prior to installation is recommended to prevent rework. The gas sample shall
be taken and analyzed as follows:
a. Isolate the pressurized component or portion of the system from the pressurized source. The recommended
hold time is not less than 24 hours.
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5.10.1.1 The component being removed and adjacent piping and equipment shall be externally cleaned with an
aqueous cleaner or NAVSEA approved halogenated solvent1 to remove loose scale, dust, dirt, and other foreign
material. Ultraviolet and white light inspections as specified in 5.13.1.2 and 5.13.1.3 shall indicate no visible
contamination.
1
For critical applications, NAVSEA approved halogenated solvents may be used for external cleaning with local
engineering approval.
5.10.1.2 That portion of the system to be entered shall be isolated with appropriate boundary isolation valves
and depressurized. Discharge of any fluid shall be in accordance with the appropriate safety precautions of
NAVSEA S9086-SX-STM-010/CH-550.
5.10.1.3 Personnel clothing, including cleanroom gloves as specified in 5.1.6, Class B, paragraph (c), or equal
shall be worn whenever handling the wetted surface of oxygen clean components. Oxygen clean component wetted
surfaces touched with bare hands shall be considered contaminated and shall be cleaned as specified in 5.2 to re-
establish oxygen cleanliness.
5.10.1.4 Systems containing oxygen at levels greater than 22 percent or hydrogen at levels greater than 3
percent shall be purged with helium or nitrogen to eliminate fire or explosion hazards using one of the following
procedures:
a. Where the configuration allows a purge path, the affected can be purged with helium or nitrogen until the
effluent purge gas measures not greater than 22 percent oxygen or 3 percent hydrogen. The measurement shall be
taken using suitable colormetric gas detector tubes such as those manufactured by Draeger Manufacturing Company
or a portable analyzer or other equivalent means.
b. Where the configuration does not allow a purge path such as a flask, or gas sampling equipment to measure
oxygen or hydrogen is not available, verify the affected area is depressurized, then pressurize to about 100 lb/in2
with helium or nitrogen, and then depressurize the affected area. Repeat the cycle one additional time for oxygen or
oxygen enriched systems for a total of two pressurization-depressurization cycles. For hydrogen systems, the
pressurization-depressurization cycle shall be performed two additional times for a total of three times. Sampling to
measure oxygen or hydrogen concentration is not required.
5.10.1.5 Only certified oxygen clean items, including replacement pipe, components, and tools, shall be
installed or come in contact with the wetted surface of an oxygen clean system or component. Oxygen clean items
removed for transportation shall be immediately packaged as specified in 5.16. If cleanliness is lost because of torn
packaging, maintenance, or repair, the effected item shall be cleaned as specified in 5.2 to re-establish oxygen
cleanliness.
5.10.1.6 Socket and seal welding in accordance with NAVSEA S9074-AR-GIB-010/278, or equal, are
considered clean processes that do not result in loss of oxygen cleanliness provided that a purge as specified in
5.10.2 is maintained. Any other welding or brazing processes result in a loss of oxygen cleanliness that requires
recleaning as specified in 5.5 or 5.8.
5.10.1.7 Establish the containment or purge requirements as specified in Table IX. When a system is opened to
remove an item, perform a visual inspection as specified in 5.13.1. Any visible contamination of the wetted surfaces
shall be locally cleaned as specified in 5.12.4. Complete the necessary maintenance and repair. Prior to closing the
system, repeat the visual inspection as specified in 5.13.1 for visual contamination. Any evidence of visible
contamination may be an indication that loss of cleanliness has occurred and additional inspections as specified in
5.12 shall be accomplished.
5.10.1.8 If there is an unscheduled delay whatsoever, such as the wrong material, an incorrect part, or
contamination, between the time that the system is opened and the time that the replacement component is installed,
the open portions of the system shall be packaged as specified in 5.16.1.3. When the system is reopened, perform a
visual inspection as specified in 5.13.1. Any evidence of visible contamination may be an indication that loss of
cleanliness has occurred and additional inspections as specified in 5.12 may be required.
5.10.2 Purge. When the system is open, a slight positive purge of about 2 lb/in2 helium or nitrogen shall be
maintained within the system to prevent possible entry of airborne contamination.
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CFC-113 or HCFC- NVR in solvent extract by gravimetric 5 ppm maximum above 5.13.2.5
225 baseline
All NAVSEA NVR in solvent by gravimetrics 5 ppm maximum above 5.13.2.6
approved baseline
halogenated solvents
All NAVSEA Residue in solvent by Optically Stimulated 5 ppm maximum above 5.13.2.7
approved Electron Emission baseline
halogenated solvents
CFC-113 Hydrocarbon oil and grease in solvent 5 ppm maximum total 5.13.2.8
extract by infrared spectrophotometry hydrocarbons
NOTES:
1/
When measuring hydrocarbon or NVR contamination, negative results are possible. These results are
acceptable and should be reported as less than 1 ppm.
2/
The preferred method of analyzing NOC is as specified in 5.13.2.3.
5.13.2.2 Shake test. A half-full capped sample container of not less than 250 mL shall be vigorously agitated
for not less than 5 seconds, then allowed to stand undisturbed for 5 minutes. Any evidence of bubbles remaining on
the surface shall be cause for rejection. The shake test is useful in detecting the presence of some soluble organic
contaminants such as hydrocarbon surfactants in low foaming inorganic solutions such as NOC. As an example,
NOC with only 5 milligrams per liter (mg/L) NID will develop a stable foam visible after 30 minutes. The presence
of foam is often the result of carry-over from a pre-clean step. However, the shake test is used only to determine the
presence of organic or particulate contamination. A shake test will not detect insoluble organic contaminants such
as oil or grease, and, therefore, shall not be used to establish the absence of organic contaminants.
5.13.2.3 Non-volatile residue in NOC. The concentration of NVR in NOC shall be determined as specified in
Appendix B.
5.13.2.4 Solvent extraction of aqueous cleaners. As specified in Appendix C, this method serially extracts a
homogenized sample of TSP solution or NOC with three 30 mL or 160 mL volumes of CFC-113 or HCFC-225, as
applicable, and subsequently dilutes the extract to either 100 mL or 500 mL. The extract is then analyzed as
specified in 5.13.2.5 or 5.13.2.8.
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5.13.2.5 Solvent extract non-volatile residue. Non-volatile residue (NVR) of solvent extract shall be
determined in accordance with ASTM F331 (see 6.3). This method evaporates 500 mL of solvent to 20 to 30 mL
using a rotary flash evaporator, evaporates the 20 to 30 mL residue with a 105 to 110 °C oven, cools the sample, and
then weighs the remaining residue, recording the NVR in ppm. Because of the volume, expense, and effluent
discharge associated with the solvent NVR analysis, activities should implement methods to collect and recycle
evaporated solvent.
5.13.2.6 Solvent non-volatile residue. Non-volatile residue (NVR) of solvent shall be determined in
accordance with NAVSEA ST700-F1-PRO-010, Appendix E, or ASTM D2109, method A (see 6.3). NAVSEA
ST700-F1-PRO-010, Appendix E, was developed for instruments that have a smaller sample size of 100 mL.
5.13.2.7 Solvent optically stimulated electron emission. Residue in solvent shall be determined in accordance
with Appendix D.
5.13.2.8 Solvent infrared spectrophotometry. Hydrocarbon oil and grease in trichlorotrifluoroethane (CFC-
113) shall be determined in accordance with ASTM D3921 (see 6.3).
5.13.2.9 White light visual clarity inspection. Samples shall be visually inspected for clarity. Inspections shall
be performed by a person with normal visual acuity, natural or corrected, under bright white light of at least 100
foot-candles. A general purpose, two D-cell flashlight in good condition, at a distance of no greater than 18 inches
directly above a surface will illuminate the surface with an intensity of not less than 100 foot-candles. Samples shall
be inspected in a chemically compatible clear container, or clean white dish. Any visible turbidity from
contaminants such as oil, grease, sediment, paint chips, bead blast, or resin beads shall be cause for rejection.
Evidence of not greater than 3 particles is acceptable.
5.13.3 Particulate inspection methods.
5.13.3.1 Applicability. Unless otherwise specified, a white light visual particle inspection as specified in
5.13.3.2 shall be performed on a sample of the final rinse water or solvent. For critical applications, a particle count
as specified in 5.13.3.3 shall be performed on a sample of the final rinse water or solvent.
5.13.3.2 White light visual particle inspection. Samples of final rinse water or solvent shall be visually
inspected for particulate contamination. Inspection shall be performed by a person with normal visual acuity,
natural or corrected, under bright white light of at least 100 foot-candles. A general purpose two D-cell flashlight, in
good condition, at a distance of not greater than 18 inches directly above a surface will illuminate the surface with an
intensity of not less than 100 foot-candles. Samples shall be inspected in a chemically compatible clear container or
clean white dish. Any visible particles shall be cause for rejection. This visual inspection corresponds to a
quantitative limit of no particles greater than 50 micrometers.
5.13.3.3 Particle count. Particle counts of final rinse water or solvent samples should meet IEST-STD-CC1246
cleanliness level 100 or 200 when determined in accordance with ASTM F311 (see 6.3). A particle count is
determined by filtering a sample of rinse water or solvent through a 1.0 micrometer, or less, membrane filter. The
size and quantity of particles on the filter is then determined using a microscope. The particle count should be
reported in relation to a known volume (1 liter) or surface area [1 square foot (ft2)] using the appropriate IEST-STD-
CC1246 cleanliness level distribution. Note that the analysis should be performed in a clean environment to prevent
contamination. One alternative to simplify the particle count is to look for a particle larger than the largest particle
size allowed to have an unlimited quantity. As an example, if the largest particle size allowed to have an unlimited
quantity is 50 micrometers, look only for particles greater than 50 micrometers. A complete particle count would be
required only if particles greater than 50 micrometers were observed.
5.13.4 pH analysis.
5.13.4.1 Applicability. When specified, the pH of rinse water shall be determined as specified in 5.13.4.2. The
pH of NOC should be determined as specified in 5.13.4.3.
5.13.4.2 Rinse water pH. When specified, the pH of rinse water shall be determined using a pH probe, litmus
paper, or phenolphthalein indicator solution. Three drops of phenolphthalein indicator solution in a 100 mL sample
will appear colorless or a very slight pink when the pH is 8.0 or less.
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5.13.4.3 NOC pH. To accurately measure the pH of NOC, measure pH as specified by MIL-DTL-24800, or
measure in accordance with ASTM E70 and the following:
a. Select a pH probe with a low sodium ion error and Teflon junction that is rated for a pH range of 0 to 14.
The Teflon junction will not clog as quickly as the commonly used ceramic junction. Use of thick glass pH probes
rated at 0 to 12 will result in pH errors of up to 0.5 units. Alternatively, an ion selective field effect transistor
(ISFET) probe can be used. The ISFET probe eliminates the pH sensitive glass tip easing clean up and extending
life.
b. Check the calibration of the pH meter with pH 10 and pH 12 buffer solutions. The common practice of
checking pH meter calibration with pH 7 and pH 10 buffer solutions will not yield accurate results.
c. After measuring the pH of NOC, clean the probe by soaking in a saturated solution of calcium hydroxide
for about 1 hour. A saturated solution of calcium hydroxide can be prepared by mixing 0.2 gm calcium hydroxide
with 100 mL of water. The presence of some precipitate indicates the solution is saturated.
5.13.5 NOC alkalinity. When specified, the alkalinity (hydroxide concentration) in NOC shall be evaluated as
follows:
5.13.5.1 Equipment.
a. A balance accurate to 0.01 grams with a zero drift less than 0.01 grams, and a capacity sufficient to prepare
reagent solutions as specified in 5.13.5.3. Suitable balances are available through laboratory supply houses such as
Thomas Scientific.
b. Beakers or erlenmeyer flasks of 100 to 250 mL capacity, plastic or glass; or equal.
c. Graduated cylinder of 50 to 100 mL capacity, plastic or glass; or equal.
d. Eye dropper or pipette, plastic or glass; or equal.
e. Syringe or buret, 35 to 50 mL capacity, with 1 mL graduation intervals, preferably plastic; or equal.
5.13.5.2 Reagents.
a. Potassium acid phthalate or potassium biphthalate (KHP), CAS No. 877-24-7, primary standard or
acidimetric standard, crystals, ACS reagent grade or better, available from chemical supply houses such as Sigma
Chemical Co. (800) 325-3010. Do not use powdered KHP; powdered KHP will not completely dissolve.
b. Thymolphthalein, pH indicator, CAS No. 125-20-2, powder, available from chemical supply houses such as
Sigma Chemical Co. (800) 325-3010.
c. Grade B water.
d. Isopropyl alcohol as specified in 4.4.2.
5.13.5.3 Reagent preparation.
a. Prepare a 4 percent wt/vol KHP solution by adding 100.0±1.0 mL of Grade B water to each 4.0±0.1 grams
of KHP (see 5.13.5.2(a)). The KHP may not dissolve in the water immediately. After adding the water to the flask
gently swirl or stir the contents for about 1 minute being careful not to deposit solid KHP on the sides of the
container. Let the container stand for 10 minutes and swirl or stir the flask for an additional minute. The KHP
solution has a 3-month shelf life when stored in a tightly sealed glass container.
b. Prepare a 0.2 percent wt/vol thymolphthalein pH indicator solution by adding 50.0±1.0 mL of isopropyl
alcohol (see 5.13.5.2(d)) to each 0.1±0.01 grams of thymolphthalein (see 5.13.5.2 (b)). The solution may have to sit
for up to 4 hours to allow the thymolphthalein to completely dissolve. The pH indicator should be clear, water white
with no precipitate. The pH indicator has a 1-month shelf life when stored in a tightly sealed brown glass or plastic
container.
5.13.5.4 Procedure.
a. Transfer 50.0±1.0 mL of the 4.0 percent KHP solution (see 5.13.5.3(a)) to the beaker or erlenmeyer flask.
b. Add five drops of the 0.2 percent thymolphthalein pH indicator solution (see 5.13.5.3(b)) to the beaker or
erlenmeyer flask. The KHP solution should be clear.
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c. Fill the syringe or buret with NOC test solution. Record to the nearest 1 mL the level of the NOC in the
syringe or buret.
d. Slowly add NOC to the KHP solution while swirling the beaker or erlenmeyer flask until a blue color
endpoint persists for 15 seconds. Record to the nearest 1 mL the final level of the NOC in the syringe or buret.
5.13.5.5 Calculation. Determine the volume of NOC used by subtracting the final level (from 5.13.5.4(d)) of
NOC solution in the syringe or buret from the initial level (from 5.13.5.4(c)) of NOC solution in the syringe or buret.
Record this volume difference in milliliters. Report this number as the alkalinity - mL of NOC. When the alkalinity
test measures 35 to 40 mL of NOC, the NOC should be discarded, or recharged as specified in 4.3.1.8.
5.13.6 Detection of hydrocarbon contamination by swipe. This procedure can be used to identify the presence
of hydrocarbons in visible contamination. Some non-visible contamination such as a film of hydrocarbon
lubricating oil may also be detected. It is intended to supplement the visual inspection methods of 5.13.1.2 to
5.13.1.4 during maintenance or loss of system cleanliness. The procedure does not measure the concentration of
hydrocarbon contamination, and shall not be used to certify cleanliness of a system or component not previously
cleaned and certified as specified in this standard. The procedure has a sensitivity of only 20 to 30 milligrams per
square foot (mg/ft2) hydrocarbons. Systems and components cleaned and certified as specified in this standard have
hydrocarbon cleanliness levels of 3 mg/ft2 or less.
5.13.6.1 Equipment.
a. Disposable pure Teflon membrane filters as specified in B.5(c) of Appendix B. Do not use bonded or
laminated Teflon filters as these filters contain hydrocarbons that will interfere with the analysis.
b. A Fourier transform infrared (FTIR) spectrometer.
5.13.6.2 Swipe Procedure.
a. Using cleanroom gloves as specified in 5.1.6, swipe the area of interest by applying direct pressure to the
center of the filter using only one finger and draw for a distance of about 1 to 2 inches. Unlike 5.13.1.4, the swipe
area is intended to be very small. In order to detect contamination with the FTIR, it is very important to locate the
contamination in the center of the filter in a very small area; preferably less than 10 millimeter diameter.
b. Transfer the filter to a non-contaminating container such as a clean polyethylene bag as specified in 5.16, or
a clean glass or clear hard plastic container. Record the date and the swipe location, and transport to a laboratory for
analysis.
5.13.6.3 FTIR Procedure.
a. Perform about 32 scans of the center swiped area of the filter with the FTIR in absorbance mode with Res 4
and full aperture between 2600 cm-1 and 3400 cm-1.
b. Review the spectrum for absorbance peaks occurring at the CH stretch region near 2930 cm-1. Absorbance
peaks in this region that are 3 to 5 times higher than background are discernable significant peaks that indicate the
presence of hydrocarbon contamination requiring corrective action.
5.14 Personnel qualification and training.
5.14.1 Applicability. Piping systems and components to be certified oxygen clean, shall be cleaned, assembled,
tested (if cleanliness is being maintained), packaged, and, when required by Table XII, inspected or witnessed by
qualified personnel. Government personnel shall be qualified as either Certified Oxygen Clean Instructors or
Certified Oxygen Clean Workers. Qualification shall be obtained by completing the appropriate course of
instruction specified in 5.14.2 and passing a written examination. Contractor personnel shall demonstrate equivalent
training by completing the appropriate course of instruction specified in 5.14.2, or its equivalent, and passing an
appropriate written examination. Vendor personnel should obtain equivalent training from authorized government
facilities or commercial agencies such as ASTM subcommittee G-4 or CGA.
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c. Intimate packaging. After performing step (a) or (b), if applicable, place the component in a film bag and
gently compress the bag to force out excess air. Heat seal the bag. For temporary closures, such as maintaining
cleanliness of a component during transport, tape may be used to completely seal the bag opening provided the
adhesive does not come in contact with the cleaned component.
d. Environmental packaging. After performing step (c), package the component using the same methods as
specified in step (c).
5.16.1.3 Internally cleaned items. If feasible, plugs or external caps should be used. Film can be used when
openings cannot be sealed with caps or plugs. Film should not be used for flasks because it may not provide an
adequate moisture barrier. The requirements are as follows:
a. Plugs and external caps. Plugs and caps shall have the same or higher degree of cleanliness as the item
being sealed. Threaded plugs shall be manufactured from brass, copper-nickel, or nickel-copper. Mechanically
expandable, insert type plugs fabricated from nonshedable rubber in accordance with ZZ-G-710, or equal, are
acceptable. The use of wood or plastic plugs is not permitted. Caps shall be fabricated from nonshedable plastic or
corrosion-resistant metal such as stainless steel, monel, brass, or copper. Caps shall be secured and sealed by bolting
or by taping. Tape or wood shall not be used as the capping material. Wood, however, may be used over the
metallic cap for purposes of bolting.
b. Closure with film. Apply a double layer of film as specified in Table XI over openings. Secure each layer
of film with a minimum of two tight wraps of tape. The tape shall not contact the open portions of the item. If the
closure is for other than temporarily maintaining cleanliness, a third layer of packaging material shall be applied in
the same manner or, preferably and if practical, completely wrap the item with packaging material as specified in
5.16.1.2.
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5.16.2 Identification.
5.16.2.1 Acceptance. In order to identify materials and components which have been certified oxygen clean, a
sticker or tag indicating certification shall be completed. The sticker or tag shall be affixed to the capped or plugged
item or package or placed between the intimate and environmental packaging containing the item so that it will not
come in contact with the certified oxygen clean item. The sticker or tag shall, at a minimum, contain the information
given on Figures 1 and 2. The shape of the tag is optional.
5.16.2.2 Rejection. In order to identify materials and components, once certified oxygen clean, which have
become contaminated and which are no longer certified oxygen clean in accordance with the provisions of this
standard, action shall be taken by the shop processing the material or quality assurance office representative to
clearly indicate that the material requires recleaning.
5.16.3 Storage.
5.16.3.1 Location. Materials and components which have been certified oxygen clean shall be stored in a clean
storage area. Certified oxygen clean materials shall be stored so as to prevent damage to their protective plastic
covers. The storage area should protect the material from exposure to dirt and oil, and should also protect the
material from temperature extremes of below 40 °F and above 100 °F. The certification sticker or tag shall be
attached so as to be visible for inspection.
5.16.3.2 Inspection of packaging. Prior to use or transport, the packaging of all certified oxygen clean materials
shall be inspected. If the outer package is torn or damaged, but the inside package is intact, replace the outer
package. If the inside package is torn or damaged exposing the oxygen cleaned surface to the ambient atmosphere,
the item shall be recleaned and recertified as specified herein. An exception is high valued items such as valves,
regulators, and compressors of which local engineering approval to use 5.12 shall be obtained (see 6.3). For
shipboard storage, the packaging of all certified oxygen clean material should be inspected every 3 years to ensure
ready spares are available.
5.17 In-process inspections.
5.17.1 Inspection. When required by Table XII, an inspector or witness shall observe the applicable operation
for compliance with this standard. The witness or inspectors shall be designated by the local activity.
5.17.2 Objective quality evidence (OQE). Objective quality evidence testifying to the satisfactory
accomplishment of the following inspections required by this standard shall be recorded and maintained for not less
than 3 years. An exception is that OQE is not required for inspections specified in 5.10 during maintenance of
cleanliness when performed by Type Commander or Ships Force personnel on systems and equipment not certified
by NAVSEA SS800-AG-MAN-010/P-9290, NAVSEA SS521-AA-MAN-010, or NAVSEA 0924-LP-062-0010.
a. Cleanroom maintenance inspections required by 5.1.2.
b. Results of testing specified by 5.9.
c. Results of inspections or analyses addressed in 5.13 when directed by this standard.
d. Signature or initial of witnesses or inspectors when directed by 5.17.1.
5.17.3 Audit or surveillance. Facilities performing oxygen cleaning may be subject to audits or surveillance
made by higher level organizations such as an assurance office representative, an authorized representative of
NAVSEA, or the agency concerned for compliance with this standard in accordance with NAVSEA TL855-AA-
STD-010. Audit or surveillance results shall be recorded (see 6.3).
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5.17.4 Accountability of small items. For most applications, measures to prevent entry of small items into
openings are adequate; however, for applications such as oxygen-nitrogen plants, accountability of small items is
also necessary. To prevent entry of small items into systems or components, attach the item to the user or to a fixed
piece of equipment by a wire, lanyard, or equivalent method. When accountability is needed, a formal written
record shall be maintained for tools, equipment, and temporary plugs or seals which are small enough to fit inside
openings in systems or components and which are used in fabrication and assembly operations, unless internal
surfaces can be visually observed and are certified to be satisfactorily clean prior to closure of the system or
component involved. A physical boundary shall be established to implement accountability when accountability is
required. Care shall be taken when establishing the physical boundary so that it precludes the inadvertent
introduction of foreign materials and tools. Extraneous tools, equipment, and material shall be removed from the
proximity of an opening in a system or component.
6. NOTES
(This section contains information of a general or explanatory nature that may be helpful, but is not mandatory.)
6.1 Intended use. This standard practice is for the precision cleaning and testing of naval surface ship,
submarine and diving oxygen, oxygen enriched systems, and interfacing systems. The precision cleaning process
specified herein is based on the processes and data reported in COMNAVSEA ltr’s Ser 03Y2A/081 dtd 24 Mar 94,
Ser 03Y2A/122 dtd 7 Apr 95, and Ser 03Y2A/275 dtd 11 Sept 95, and supplements thereof; and NASA Doc. No.
WSTF-IR-95-0048 dated 30 Jan 95, and supplements thereof. The performance of the precision cleaning process
specified herein directly affects the safe operation of naval surface ship, submarine and diving oxygen systems,
oxygen enriched systems, and interfacing systems. Nonconformance can result in the introduction or failure to
remove toxic and flammable contaminants that can cause catastrophic equipment failure and personnel injury and
death.
6.2 Acquisition requirements. Acquisition documents should specify the following:
a. Title, number, and date of the standard.
b. Identification of critical application systems or components as defined in 3.11, if applicable.
6.3 NAVSEA approval and direction.
6.3.1 Deviations from specified materials, procedures, and requirements and selection of specific alternative
materials and procedures require NAVSEA approval or direction. Requests should include supporting
documentation.
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6.3.2 Several referenced documents within Appendix A of this standard are known to be officially withdrawn at
the time of this revision’s approval. Since these documents are still in common use within commercial practice and
industry, the official status of these publications should not affect the intent of this specification. Additionally, three
documents that have been officially withdrawn at the time of this revision’s approval are still in common use within
commercial practice and industry; and continued use is technically acceptable. FED-STD-209, Airborne Particulate
Cleanliness Classes in Cleanrooms and Clean Zones, has been cancelled and replaced by ISO-14644 (reference
Section 5.1). However, FED-STD-209 Class 100,000 (or better) clean rooms for critical applications are technically
acceptable alternatives to ISO-14644. MIL-STD-1246 has been cancelled and replaced by IEST-STD-CC1246
(reference Section 5.13). However, particle counts in accordance with MIL-STD-1246, Product Cleanliness Levels
and Contamination Control Program, for critical applications are technically acceptable alternatives to IEST-STD-
CC1246. ASTM D930, Standard Test Method of Total Immersion Corrosion Test of Water Soluble Aluminum
Cleaners, has been cancelled without replacement (Reference Appendix A). For historical purposes, ASTM D930
was used to evaluate the corrosion resistance of all aqueous cleaners with aluminum.
6.4 Safety precautions. If an oxygen monitor with alarm is used as specified in 4.7.1, it should be in
accordance with OPNAVINST 5100.19.
6.5 Subject term (key word) listing.
Halogenated solvent
Helium
Hydrogen
Isopropyl alcohol
Navy oxygen cleaner (NOC)
Oxygen
Oxygen clean
Trisodium phosphate
6.6 Change notations. The margins of this standard are marked with vertical lines to indicate modifications
generated by this change. This was done as a convenience only and the Government assumes no liability
whatsoever for any inaccuracies in these notations. Bidders and contractors are cautioned to evaluate the
requirements of this document based on the entire content irrespective of the marginal notations.
1/ 2/
Name: ________________ Date: _____________
3/ 4/
Final Cleaner: __________ Control No: _________
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CERTIFIED
OXYGEN CLEAN MIL-STD-1330
WARNING: DO NOT OPEN
UNTIL READY FOR USE
1/
Name: _____________________________
2/
Date: ______________________________
3/
Final Cleaner: _______________________
4/
Control No: _________________________
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MIL-STD-1330D(SH)
APPENDIX A
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MATERIAL COMPATIBILITY
A.1 SCOPE
A.1.1 Scope. This Appendix is a mandatory part of the standard. The information contained herein is intended
for compliance. This appendix provides results of compatibility testing and direction for performing additional
testing.
A.2 APPLICABLE DOCUMENTS
A.2.1 General. The documents listed in this section are specified in sections A.3 of this standard. This section
does not include documents cited in other sections of this standard or recommended for additional information or as
examples. While every effort has been made to ensure the completeness of this list, document users are cautioned
that they must meet all specified requirements of documents cited in sections A.3 of this standard, whether or not
they are listed.
A.2.2 Non-Government publications. The following documents form a part of this document to the extent
specified herein. Unless otherwise specified, the issues of the documents are those cited in the solicitation or
contract (see 6.2).
A.3 PROCEDURE
A.3.1 Compatibility testing. Compatibility is determined by evaluating material properties such as weight,
volume, tensile strength, elongation, or hardness and, for metals, inspecting the surface for discoloration and
degradation after exposure to the fluid of interest. Guidelines for performing material compatibility testing are as
specified in A.3.2 through A.3.4. These guidelines are conservative. Accordingly, local engineering review of
compatibility testing performed or actual experience may result in different conclusions. Results of compatibility
testing using these guidelines are provided in Tables A-I through A-III. If experience or testing indicates that a
material is less compatible than as indicated in these tables, contact NAVSEA. If a material of interest is not listed
in these tables, compatibility testing shall be accomplished using the following guidelines.
A.3.2 Metal. ASTM D930 or ASTM D1280 provide guidance for performing compatibility testing on metals.
The allowable corrosion limits are as specified in MIL-DTL-24800.
A.3.3 Rubber. ASTM D471 or ASTM D1414 provide guidance for performing compatibility testing on
rubbers. The criteria to determine the exposure limits are as specified in Table A-IV.
A.3.4 Plastic. ASTM D543 provides guidance for performing compatibility testing on plastics. The criteria to
determine the exposure limits are as specified in Table A-V.
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APPENDIX A
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APPENDIX A
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MIL-STD-1330D(SH)
APPENDIX A
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TABLE A-III. Plastic material compatibility.
NOC TSP WATER
PLASTIC; specification NID 1/ 2/
170 °F 1/ 170 °F 1/ 170 °F 1/
ABS, Acrylonitrile butadiene styrene; Commercial C C C NH
DELRIN, Acetal resin; ASTM D4181 C C C C
EPOXY, Epoxy resin; Commercial, unfilled I I I C
HDPE, High density polyethylene; ASTM D1248 C C C C
LEXAN, Polycarbonate resin; Commercial C C C C
LUCITE & PLEXIGLASS, Methyl-methacrylate; I 1L 1L C
MIL-P-5425, finish A
NYLON, Polyamide resin; ASTM D4066, nylon 6,6 1L 1L 1L 1L
PAI, Polyamide-imide (Torlon 4203L); Commercial, injection 12L 12L C NH
molded
PEI, Polyetherimide (Ultem 1000); Commercial, injection molded 1L 1L C C
Polyurethane; Commercial 12L C I NH
PP, Polypropylene; ASTM D4101, unfilled 12L C C C
PVC, Polyvinyl chloride; ASTM D1784, rigid C C C C
PVC, Polyvinyl chloride; ASTM D2287, nonrigid 12L C 12L C
SURLYN, Ionomer resin; Commercial, No. 9650 NT I I C
SURLYN, Ionomer resin; Commercial, No. 9720 I C C C
TEFLON FEP, Fluoethyl propylene; ASTM D2116 C C C C
TEFLON TFE, Polytetrafluoro-ethylene; ASTM D1457 12L 12L C C
VESPEL-21, Polyamide resin + graphite; Commercial 1L 1L NT C
NOTES:
1/
“C” indicates that the material is compatible with the cleaning agent.
“I” indicates that the material is not compatible with the cleaning agent.
“1L” indicates that exposure of the material should be limited to 1 hour per cleaning.
“12L” indicates that exposure of the material should be limited to 12 hours per cleaning.
“C/D” indicates that the material is compatible with the cleaning agent, but the material surface was
discolored during testing. Testing on a sample of the material may be necessary to determine if the
discoloration is permissible.
“NT” indicates that the material was not tested.
2/
Compatibility of NID is based on test data and service history. “NH” indicates that there is no test data or
history on the material compatibility.
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APPENDIX A
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APPENDIX B
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MIL-STD-1330D(SH)
APPENDIX B
w/ Change 1
d. Stainless steel vacuum filtration column with not less than 250 mL capacity available from laboratory
supply houses such as Fischer Chemical is preferred. Alternately, an inexpensive Teflon vacuum or pressure
filtration reservoir of 250 mL capacity minimum is available from Savillex Corp., 6133 Baker Rd, Minnetonka, MN
55345, (612) 935-4100, consisting of cap with connection for 1⁄4-inch tube, part number 501-4; upper segment, part
number 504; lower segment, part number 504-47; and upper/lower segment connector, part number 502, or equal.
e. Laboratory homogenizer with 500-1000 watt motor power with a no-load speed control of 10,000 to 30,000
revolutions per minute (rpm), and a 20 millimeter diameter saw tooth generator capable of homogenizing a 1 liter
sample into a 1-5 micrometer emulsion at about 7,500 rpm loaded speed. Suitable homogenizers and generators are
available from Omni International Inc., 6530 Commerce Court, Gainesville, VA (800)776-4431, homogenizer part
number GLH-115 and generator part number G20-195ST; or PRO Scientific, PO Box 448, Monroe, CT (203)452-
9431, homogenizer part number 01-01250 and generator part number 02-20200. A holder or stand for the
homogenizer is recommended.
f. A drying oven capable of maintaining a temperature of 55 °C (131 °F) to 60 °C (140 °F).
g. NOC sample/homogenizing bottles of 1-liter volume for collecting and homogenizing NOC effluent from
oxygen systems or NOC effluent from oxygen components. Ensure the opening is large enough to allow insertion of
the homogenizer generator (item (e)). Wide mouth glass sample bottles with external safety coatings and Teflon
lined caps are acceptable, as are sampling containers manufactured from Teflon, Teflon lined glass, Teflon lined
plastic, or stainless steel. Suitable containers are available from laboratory supply houses such as Thomas Scientific.
h. Graduated cylinders of 250 mL minimum volume with minimum graduations of 50 mL to measure 200 mL
of homogenized NOC sample to be filtered. Cylinders should be glass or polypropylene.
i. A vacuum collector of 500 mL capacity to collect filtered NOC when using a vacuum to draw the NOC
through the membrane filter, preferably made of plastic. The stopper used to seal the collector should be made of
Teflon. The stopper requires a 1⁄4-inch outside diameter hole for the tube from the filter support.
j. Beakers of 250 mL capacity to collect the filtered NOC, preferably plastic, when pressurizing the NOC
sample.
k. Beakers of 250 mL capacity to measure 100 mL of demineralized water used to wash the membrane filter.
l. Erlenmeyer flasks of 1 liter capacity, plastic or glass, for rinsing the homogenizer. Ensure the opening is
large enough to allow insertion of the homogenizer generator (item (e)).
m. Petri dishes, quantity 2, which are covered, glass and 50 millimeter minimum diameter for drying
membrane filters in the oven.
n. Forceps with non-serrated tips to handle filters.
o. An eye dropper or pipette to transfer isopropyl alcohol to wet the membrane filter prior to filtration.
p. Teflon tape to prepare threaded connections on the filtration reservoir.
q. If using a vacuum to draw the NOC through the membrane filter, a vacuum source capable of drawing a
vacuum equivalent to 10 inches Hg (5 lb/in2 differential) and controllable at 2 inches Hg (1 lb/in2) increments.
Sources of vacuum include traditional electric vacuum pumps; gas vacuum ejector pumps available from Cole-
Parmer, and inexpensive water aspirator/ejector vacuum pumps such as Nalgene Part No. 6140-0010.
r. If using pressure to push the NOC through the membrane filter, an oil-free air or nitrogen pressure source
capable of providing 5 lb/in2 and controllable at 1 lb/in2 increments.
B.6 Reagents.
a. Navy oxygen cleaner (NOC) in accordance with MIL-DTL-24800.
b. Demineralized water in accordance with ASTM D1193 Type II or 1 micrometer nominal filtered Grade B
as specified in 4.2.
c. Isopropyl alcohol, American Chemical Society (ACS) reagent grade, having an NVR of 5 ppm (0.005
percent) or less which is available from laboratory supply houses.
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MIL-STD-1330D(SH)
APPENDIX B
w/ Change 1
B.7 Samples.
a. A 500 to 600 mL sample of new-unused NOC shall be collected from each container or drum of each lot or
batch to establish a baseline NVR.
b. A 500 to 600 mL NOC sample of the NOC effluent from the oxygen system or component being cleaned
shall be collected for cleanliness verification.
c. Samples of homogenized NOC used for the gravimetric analysis will be 200 mL.
B.8 Preparation and maintenance of apparatus.
B.8.1 Apparatus used in the procedure, including the sample bottles, homogenizer, homogenizing container,
graduated cylinder, filtration reservoir, and demineralized water beaker shall have been cleaned as specified in 5.2.
B.8.2 Threaded connections in the filtration reservoir and filter support shall be wrapped with Teflon tape to
prevent leakage of the NOC sample.
B.8.3 After contact with NOC, all apparatus shall immediately be rinsed with demineralized water to remove
residual NOC to prevent formation of inorganic deposits and to maintain cleanliness.
B.9 Procedure.
B.9.1 Select a membrane filter that has equilibrated to ambient conditions.
B.9.2 Using forceps, weigh the filter to the nearest 0.1 mg, preferably to the nearest 0.05 mg.
B.9.3 Transfer the membrane filter to the filter holder and attach the filter holder to the filtration reservoir as
shown on Figure 3. DO NOT OVER TIGHTEN. Over tightening the threaded connections may cause permanent
deformation allowing the NOC sample to leak.
B.9.4 Homogenize the 500 to 600 mL NOC sample for 3 minutes at a speed of about 7,500 revolutions per
minute (rpm) (position 3 on an OMNI Model GLH homogenizer).
B.9.5 Using an eye-dropper or pipette, wet the filter with about 1 mL of isopropyl alcohol. Allow not less than
15 seconds for the isopropyl alcohol to fully wet the filter. This is observable as a change in filter color from opaque
white when dry to translucent when wet.
B.9.6 Optional - Excessive isopropyl alcohol can react with NOC to form a white precipitate that may cause
high NVR results. If this interference is suspected, the isopropyl alcohol can be removed from the filter by
transferring 15 to 25 mL of demineralized water to the filter reservoir and filtering the demineralized water by
vacuum or pressurizing the reservoir with oil-free air or nitrogen before proceeding to step B.9.7.
B.9.7 Transfer 200 mL of homogenized NOC to the filter reservoir.
B.9.8 Filter the homogenized NOC at less than 50 mL/min by vacuum or by pressurizing the reservoir with oil-
free air or nitrogen. Very little pressure differential (less than 5 psid) will be required to obtain the desired filtration
rate. DO NOT EXCEED A FILTRATION RATE OF 50 MILLILITERS PER MINUTE.
B.9.9 Transfer 100 to 110 mL of demineralized water to the filter reservoir to wash the filter and reservoir of
residual NOC.
B.9.10 Filter the demineralized water at less than 50 mL/min by vacuum or by pressurizing the reservoir with
oil-free air or nitrogen. Very little pressure differential (less than 5 psid) will be required to obtain the desired
filtration rate. DO NOT EXCEED A FILTRATION RATE OF 50 MILLILITERS PER MINUTE.
B.9.11 Remove the filter, place in a petri dish, and dry with petri dish cover ajar in an oven at 131 to 140 °F (55
to 60 °C) for 20 to 30 minutes.
B.9.12 Remove the petri dish with filter from the oven, transfer the filter to an ambient temperature petri dish,
and allow it to cool with the cover ajar for at least 2 minutes.
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MIL-STD-1330D(SH)
APPENDIX B
w/ Change 1
B.9.13 Weigh the filter to the nearest 0.1 mg; preferably to the nearest 0.05 mg.
B.10 Calculations.
B.10.1 Calculate the baseline (before use) NVR in NOC by subtracting the initial weight of the filter (step
B.9.2) from the final weight of the filter (step B.9.13) after filtering new-unused NOC. Record the weight difference
in mg. Multiply the weight difference by five, and record as baseline (before use) mg/L NVR in NOC.
B.10.1.1 Perform a baseline analysis for each lot or batch of NOC. The term lot or batch refers to the
manufacturing lot or batch numbers identified on each container of NOC. Where multiple containers have the same
lot or batch number, only one container needs to be sampled. For cleaning applications using multiple containers
with different lot or batch numbers, either the average of the different baselines or the lowest of the different
baselines shall be used when determining final NVR in NOC.
B.10.1.2 When determining baseline NVR in new-unused NOC, step B.9.4 may be deleted, and
unhomogenized NOC may be used in step B.9.7.
B.10.2 Calculate the post-cleaning (after use) parts per million (ppm) above baseline NVR in NOC as follows:
B.10.2.1 Subtract the initial weight of the filter (step B.9.2) from the final weight of the filter (step B.9.13) after
filtering used NOC. Record the weight difference in mg. Multiply the weight difference by five, and record as
post-cleaning (after use) mg/L total NVR in NOC.
B.10.2.2 Subtract the baseline (before use) NVR (from stepB.10.1) from the post-cleaning (after use) total
NVR (from step B.10.2.1). Record the difference as post-cleaning (after use) mg/L above baseline NVR in NOC.
B.10.2.3 Convert mg/L to ppm by dividing mg/L (from step B.10.2.2) by 1.075 (the average density of NOC in
use) and record as ppm above baseline NVR in NOC.
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MIL-STD-1330D(SH)
APPENDIX B
w/ Change 1
NITROGEN GAS
SOURCE
CAP
UPPER COLUMN
SOILED NOC
UNION
LOWER COLUMN
FILTER HOLDER
WITH FILTER
VACUUM
SOURCE
FILTERED
NOC
PRESSURIZATION VACUUM
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MIL-STD-1330D(SH)
APPENDIX C
w/ Change 1
TEST PROCEDURE FOR SOLVENT EXTRACTION OF AN AQUEOUS INORGANIC CLEANER
C.1 SCOPE
C.1.1 Scope. This appendix is a mandatory part of the standard. The information contained herein is intended
for compliance. This appendix provides a procedure for solvent extraction of inorganic aqueous Navy oxygen
cleaner (NOC) or tri-sodium phosphate (TSP) cleaning solution. The solvent extract is subsequently analyzed for
hydrocarbon oil and grease or non-volatile residue.
C.2 APPLICABLE DOCUMENTS
This section is not applicable to this appendix.
C.3 PROCEDURE
C.3.1 Summary of test method. The solvent extraction is performed by serially extracting a 500 mL
homogenized sample of NOC or TSP with three 160 mL volumes of CFC-113 or HCFC-225 if analyzing for non-
volatile residue (NVR) by gravimetric, or serially extracting a 100 mL homogenized sample of NOC or TSP with
three 30 mL volumes of CFC-113 solvent if analyzing for hydrocarbon oil and grease by infrared
spectrophotometry. Extracts analyzed for NVR are subsequently diluted to 500 mL, while extracts analyzed for
hydrocarbon oil and grease by infrared spectrophotometry are subsequently diluted to 100 mL.
C.4 Significance and use.
C.4.1 NOC in accordance with MIL-DTL-24800 and TSP in accordance with O-S-642 are aqueous inorganic
solutions that generally contain less than 1 ppm solvent extractable material. NOC and TSP remove industrial oils
and greases by displacement with the resultant removed insoluble contaminants existing as a suspension. When
mixed with a solvent, the solvent extracts the oil and grease for post hydrocarbon oil and grease or NVR analysis
depending upon the solvent used. Since HFE-7100 has marginal hydrocarbon solvency, it cannot be used for
extraction.
C.4.2 All NAVSEA halogenated solvents are denser than NOC or TSP solutions so the solvent will settle to the
bottom of a separatory funnel during an extraction process.
C.4.3 This test method does not acidify the NOC aqueous sample to a pH of 2 or less like common waste water
analyses. Soluble organic materials that would be detectable when acidifying to a pH of 2 are easily detected as a
stable foam when performing the shake test as specified in 5.13.2.2.
C.4.4 The homogenizing process cleans oil and grease from the sides of the sample container and equally
distributes insoluble oil and grease through the sample as a fine emulsion. This ensures that samples drawn from the
original 500 to 600 mL sample are representative.
C.4.5 During the extraction process, small quantities of aqueous cleaner solution will be captured by the
solvent. The non-volatile inorganic constituents of the captured aqueous cleaner can interfere with subsequent NVR
analyses. This interference can be avoided by establishing a baseline NVR analysis of the aqueous cleaner.
C.5 Apparatus.
a. Laboratory homogenizer with 500-1000 watt motor power with a no load speed control of 10,000 to 30,000
revolutions per minute (rpm), and a 20 millimeter diameter saw-tooth generator capable of homogenizing a 1 liter
sample into a 1-5 micrometer emulsion at about 7,500 rpm loaded speed. Suitable homogenizers and generators are
available from Omni International Inc., 6530 Commerce Court, Gainesville, VA (800)776-4431, homogenizer part
number GLH-115 and generator part number G20-195ST; or PRO Scientific, PO Box 448, Monroe, CT (203)452-
9431, homogenizer part number 01-01250 and generator part number 02-20200. A holder or stand for the
homogenizer is recommended.
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MIL-STD-1330D(SH)
APPENDIX C
w/ Change 1
b. Sample/homogenizing bottles of 1 liter volume for collecting and homogenizing NOC or TSP samples.
Ensure the opening is large enough to allow insertion of the homogenizer generator (item (a)). Wide mouth glass
sample bottles with external safety coatings and Teflon lined caps are acceptable, as are sampling containers
manufactured from Teflon, Teflon lined glass, Teflon lined plastic, or stainless steel. Suitable containers are
available from laboratory supply houses such as Thomas Scientific.
c. Graduated cylinders of 50 mL minimum volume with minimum graduations of 10 mL to measure 30 mL of
solvent and 100 mL minimum volume with minimum graduations of 50 mL to measure 100 mL of aqueous sample,
or 250 mL minimum volume with minimum graduations of 10 mL to measure 160 mL of solvent and 500 mL
minimum volume with minimum graduations of 100 mL to measure 500 mL of aqueous sample. Cylinders should
be glass.
d. Separatory funnels of 250 mL volume minimum for extracting a 100 mL aqueous sample, or 1000 mL
minimum volume for extracting a 500 mL aqueous sample. Funnels should be glass.
e. Beakers of sufficient capacity to collect 30 mL or 160 mL serial solvent extracts and transfer to the
volumetric flask. Beakers should be glass.
f. Volumetric flasks, or equal, of 100 mL minimum volume with minimum graduations of 100 mL to collect
the three 30 mL solvent extracts, or 500 mL minimum volume with minimum graduations of 500 mL to collect the
three 160 mL solvent extracts.
C.6 Reagents.
a. Navy oxygen cleaner (NOC) in accordance with MIL-DTL-24800.
b. Tri-sodium phosphate (TSP) in accordance with O-S-642 prepared as specified in 4.3.2.
c. Hydrochloric or sulfuric acid (1+1), ACS reagent grade, prepared by slowly and carefully adding 1 volume
of hydrochloric acid (HCl) or sulfuric acid (H2SO4) to 1 volume of water.
d. CFC-113 or HCFC-225 (see Appendix E).
C.7 Samples.
a. A 500 to 600 mL NOC or TSP sample shall be collected for hydrocarbon or NVR determination. The
sample bottles used to collect the sample shall have been cleaned as specified in C.8.
b. A 500 mL sample of homogenized NOC or TSP will be used when performing a solvent extraction for post
NVR analysis by gravimetric.
c. A 100 mL sample of homogenized NOC or TSP will be used when performing a solvent extraction for post
hydrocarbon oil and grease analysis by infrared spectrophotometry.
C.8 Preparation and maintenance of apparatus.
C.8.1 When handling CFC-113 or HCFC-225, the safety precautions specified by the material safety data sheet
(MSDS) and 4.4.1 shall be followed.
C.8.2 Apparatus used in the procedure, including the sample bottles, homogenizer, homogenizing container,
graduated cylinder, filtration reservoir, and demineralized water container, shall have been cleaned using a
component cleaning process as specified in this standard, or equal.
C.8.3 After contact with NOC or TSP cleaning solution, all apparatus shall immediately be rinsed with
demineralized water to remove residual cleaner, to prevent formation of inorganic deposits and to maintain
cleanliness.
C.9 Procedure.
C.9.1 Cool the 500 to 600 mL NOC or TSP sample to room temperature or less. Acidify TSP samples to a pH
of 2 or less.
C.9.2 Homogenize the 500 to 600 mL sample for 3 minutes at a speed of about 7,500 rpm (position 3 on an
OMNI Model GLH homogenizer).
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MIL-STD-1330D(SH)
APPENDIX C
w/ Change 1
NOTE 1: CFC-113 or HCFC-225 can be used for post NVR analysis. Only CFC-113 solvent can be used for
post analysis by infrared spectrophotometry.
C.9.3 Transfer 100 mL or 500 mL of homogenized sample to the separatory funnel.
C.9.4 Transfer 160 mL of CFC-113 or HCFC-225, or 30 mL of CFC-113 to the separatory funnel. Cap and
vigorously agitate for 30 seconds. Allow to stand until contents settle and bubbles disappear. Remove the cap
carefully to release any pressure build-up. Drain solvent from separatory funnel and transfer to volumetric flask.
Repeat two additional times.
C.9.5 Add fresh solvent to the volumetric flask and dilute solvent extract to 500 mL if serially extracted with
160 mL volumes or to 100 mL if serially extracted with 30 mL volumes. Shake to completely mix the solvent
extract. Remove the cap carefully to release any pressure build-up.
C.9.6 Perform an NVR analysis of the 500 mL solvent extract as specified in 5.13.2.5, or perform a
hydrocarbon oil and grease analysis of the 100 mL solvent extract as specified in 5.13.2.8.
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MIL-STD-1330D(SH)
APPENDIX D
w/ Change 1
ANALYSIS OF RESIDUE IN SOLVENT BY OPTICALLY STIMULATED ELECTRON EMISSION USING A
SURFACE QUALITY MONITOR
D.1 SCOPE
D.1.1 Scope. This appendix is a mandatory part of the standard. The information contained herein is intended
for compliance. This appendix provides a procedure for determination of oil and grease in NAVSEA approved
halogenated solvent by optically stimulated electronic emission (OSEE).
D.2 APPLICABLE DOCUMENTS
D.2.1 General. The documents listed in this section are specified in Appendix D of this standard. This section
does not include documents cited in other sections of this standard or recommended for additional information or as
examples. While every effort has been made to ensure the completeness of this list, document users are cautioned
that they must meet all specified requirements of documents cited in Appendix D of this standard, whether or not
they are listed.
D.2.2 Government documents.
D.2.2.1 Specifications, standards, and handbooks. The following specifications, standards, and handbooks
form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these
documents are those cited in the solicitation or contract.
DEPARTMENT OF DEFENSE SPECIFICATIONS
MIL-PRF-17331 - Lubricating Oil, Steam Turbine and Gear, Moderate Service
(Copies of this document are available online at http://assist.daps.dla.mil/quicksearch/ or
http://assist.daps.dla.mil or from the Standardization Document Order Desk, 700 Robbins Avenue, Building 4D,
Philadelphia, PA 19111-5094.)
D.3 PROCEDURE
D.3.1 Summary of test method. The concentration of non-volatile organic residue in solvent is determined to
be less than, equal to, or greater than the established acceptance criteria by serially evaporating 0.5 mL of solvent in
a specially machined dish and measuring the OSEE of the dish using a Surface Quality Monitor (SQM). The
amount of solvent evaporated is determined by whether or not the baseline is applied. If the baseline is not applied,
acceptance criteria of 5 ppm or less is determined by evaporating 1.5 mL of solvent and comparing to the result of
1.5 mL of 5 ppm standard. If the baseline is applied, acceptance criteria of 5 ppm above baseline is determined by
evaporating 1.5 mL of solvent and comparing to the result of 1.5 mL of unused solvent (baseline), followed by 1.5
mL of 5 ppm standard.
D.4 Significance and use.
D.4.1 The quantitative cleanliness standard for systems cleaned as specified in this standard generally applies
to hydrocarbon non-volatile residues. However, this method does not differentiate between hydrocarbon based
products (such as TEP 2190 oil) and fluorocarbon based products (such as Krytox 240AC grease). Additionally, this
method is not sensitive to small quantities of particulate.
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MIL-STD-1330D(SH)
APPENDIX D
w/ Change 1
D.4.2 The specially machined dishes concentrate the sample to a small area that is within the focal point of the
ultraviolet light source used by the SQM. The theory of OSEE is that some very clean surfaces, such as stainless
steel, illuminated by an ultraviolet light source will emit electrons from the surface that are measurable in the form
of current. As the surface is contaminated, the electron emission decreases reducing the measured current. An
exception to this rule is that in rare instances, such as some surfactants, the current can increase. Properly machined
and cleaned evaporating dishes will measure similarly. Likewise, properly machined and cleaned evaporating
dishes when uniformly contaminated with a known standard will also measure similarly. Therefore, comparing the
results from a 5 ppm standard (with or without baseline) to the results of effluent or waste solvent can be used to
quantitatively determine a go-no-go acceptance criteria. However, the electron emission is not linear, and therefore,
empirical determination of the exact quantity of non-volatile organic residue cannot be determined by this method.
Also, if the current increases more than an established amount, it is an indication that a contaminant other than oil
and grease is present, which is considered a failure requiring recleaning.
D.4.3 Baseline can be applied as specified in Table X. The acceptance criteria of 5 ppm above baseline is
established by evaporating 1.5 mL of unused solvent (baseline) followed by 1.5 mL of 5 ppm standard. The effluent
or waste solvent is comprised of the unused solvent contaminated with as much as 5 ppm, therefore, only 1.5 mL of
this solvent is needed for the analysis.
D.4.4 This analysis method uses three different laboratory standards: 7.80 mg TEP 2190 oil in one liter of
CFC-113 or HCFC-225 solvent, and 1.75 mg Krytox 240AC grease in one liter of HFE-7100 solvent. Each standard
is applicable only to the solvent used during the actual cleaning process, except HCFC-225G and HCFC-225M can
be used interchangeably as standards, and will hereafter be referred to as HCFC-225. Consistent with previous
practice, all laboratory standards are normalized to the measured response from 5 ppm hydrocarbon oil in solvent.
For the HFE-7100 standard, Krytox 240AC grease was used as the contaminant because of its solvency in HFE-
7100. However, Krytox 240AC grease has a higher sensitivity to OSEE, and therefore requires less contaminant to
produce a measured response equivalent to 5 ppm hydrocarbon oil.
D.5 Apparatus.
D.5.1 The following is needed to perform OSEE analysis. Apparatus needed to prepare the 5 ppm laboratory
standard is not listed, but needs to be adequate to prepare the standard as specified in D.9.
a. A Surface Quality Monitor (SQM), Model SQM 200 with sensor 60262, with 0.25-inch diameter aperture
installed, for measuring residue on the evaporating dish by OSEE. The instrument can be purchased from Photo
Emission Tech., Inc., (805) 499-7667. Note that “Surface Quality Monitor” is a trade name. However, since it is
the only instrument of its kind capable of performing this type of analysis and is patented, the trade name is
commonly used.
b. Evaporating dishes manufactured per Figure 4. With a vibro-etch tool or equivalent, mark the side of each
dish with a letter or number to uniquely identify each dish.
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MIL-STD-1330D(SH)
APPENDIX D
w/ Change 1
c. A hot plate adjustable to about 90 and 100 °F with an accuracy of ±5 °F. Note that many hot plates are not
adjustable to these low temperatures, they don’t provide adequate accuracy, and adjustable plates with digital
temperature readout are costly. An acceptable hot plate is Corning catalog number 440918 available from
laboratory supply houses such as Fisher Scientific. This hot plate has a remote control that provides the required
adjustability. Rather than a digital readout of temperature, it provides a digital readout of the heat setting to the
nearest 0.1, with a maximum setting of 10. Many hot plates are only adjustable in increments of 1, with a maximum
setting of 10.
d. A washing bottle used for spraying solvent for final cleaning of glassware and displacing water from the
evaporating dishes. The bottles must not extract organics and must be compatible with the solvent, such as Teflon
or glass. An acceptable washing bottle is VWR Scientific catalog number 16651-880.
e. Glass pipet with a capacity of 0.5 mL for measuring laboratory standard. Suitable pipets are available from
laboratory supply houses such as Fisher Scientific or VWR Scientific.
f. Pipet filler/dispenser. Fisher Scientific catalog number 13-683B is acceptable.
g. Glass beaker with a capacity of 10 mL for transferring laboratory standard to evaporating dishes. The
small size is necessary to minimize solvent evaporation. Other suitable beakers are available from laboratory supply
houses such as Fisher Scientific or VWR Scientific.
h. Non-abrasive, heavy-duty, reinforced paper towels for cleaning evaporating dishes. Kimberly-Clark P/N
34865 available from Fisher Scientific catalog number 06-666-14A is acceptable. If available, stock number 7920-
00-823-9773 per A-A-1432, Type IV, is acceptable.
i. A clean container for mixing detergent for cleaning evaporating dishes. An appropriate size is about 5½
inches square and 3 inches deep with an open top. This size allows use of minimum cleaner and adequate access for
cleaning by hand. Any commercially available type is acceptable.
j. A thermometer capable of reading a surface temperature of 90 and 100±2 °F.
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MIL-STD-1330D(SH)
APPENDIX D
w/ Change 1
k. Equipment for performing maintenance on the SQM. For checking the ultraviolet lamp intensity, a
research radiometer, model IL1400 and a detector at 185 nm, model SEL185 both available from International Light
(978) 465-5923, and additionally, an adapter, part number 10528, available from Photo Emission Tech., Inc. (805)
499-7667. For checking the sensor electronics, a calibration load model #60054 available from Photo Emission
Tech, Inc. (805) 499-7667.
D.6 Reagents.
D.6.1 The following are required to prepare 5 ppm laboratory standards in a chemistry laboratory:
a. New, unused NAVSEA approved halogenated solvent that will be used as the cleaning solvent is required
to prepare laboratory standards (i.e., if HFE-7100 will be used as the cleaning solvent, then HFE-7100 must be used
to prepare the laboratory standard).
b. MS2190-TEP, MIL-PRF-17331, if preparing the HCFC-225 or CFC-113 laboratory standards.
c. Krytox Grease DuPont 240AC, MIL-PRF-27617 if preparing the HFE-7100 laboratory standards.
D.6.2 The following are required to perform OSEE analysis of solvent:
a. Sparkleen available from Fisher Scientific, catalog number 04-3204 (3.25 pounds per box). Prepare the
Sparkleen cleaning solution in a container (D.5.1(i)) by diluting with tap water per the manufacturer’s instructions.
Use of other cleaners is not allowed. Disposal shall be in accordance with local, state, and federal regulations.
b. Tap water.
c. New, unused NAVSEA approved halogenated solvent as specified in 4.4 is needed to final clean glassware
and rinse evaporating dishes. New, unused NAVSEA approved halogenated solvent is also required to prepare
laboratory standards.
D.7 Samples. The following samples are required for analysis:
a. If baseline applies, a sample of new-unused solvent of not less than 20 mL shall be collected from each
container or drum of each lot or batch.
b. A sample of solvent used as a final cleaning solvent shall be not less than 20 mL in a glass bottle with a
screw cap having a Teflon liner.
D.8 Preparation and maintenance of apparatus.
D.8.1 Setting hot plate temperature.
D.8.1.1 For the hot plate of D.5.1 (c), adjust the rheostat and measure the surface temperature of the hot plate
using the thermometer of D.5.1 (j). Continue adjusting until the desired temperature (85 to 90 °F for CFC-113 or
HCFC-225 or 90 to 100 °F for HFE-7100) is attained and stays below the maximum specified temperature for 10
minutes. Note the digital readout for each of these temperatures (e.g., 0.2 may equate to 90 °F and 0.3 may equate to
100 °F). For subsequent use of this hot plate, the hot plate can be set using the digital readout and measurement of
temperature is not necessary. The hot plate shall be checked every 3 months.
D.8.2 Set up SQM.
D.8.2.1 Turn the power to the control unit OFF. Inspect the sensor to confirm that the manufacturer installed a
0.25-inch diameter aperture. The aperture is needed so that only the horizontal surface at the center of the dish in the
evaporating area is measured.
CAUTION 1: During installation, the person installing the aperture MUST be grounded. Electrostatic
discharge can damage the sensor electronics. At a minimum, wear a properly grounded conductive wrist strap. Also
during installation, handle the apertures with the tweezers provided to prevent contamination that can seriously
degrade sensor performance.
If it was not installed, following the manufacturer’s instructions, install the 0.25-inch diameter aperture on the
sensor.
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D.8.2.2 With the dish next to (not directly under) the sensor, set the sensor so that it is slightly below the top of
the evaporating dish. This setting will provide minimum movement of the sensor when sliding the dish under it.
The micrometer reading is not important and can be changed provided that the sensor is set slightly below the top of
the evaporating dish so that it will sit flush on the dish when taking a reading. For information, the micrometer on
the stand can be used to set the sensor at a specified distance from the bottom of the stand. The purpose of this is to
provide a means of attaining a consistent standoff distance from the sample being measured. The sensor can be
moved up from this point, but when moved back down, it will end up at this point. The application in this appendix
is different in that when taking a reading, the sensor is moved up, the dish is placed under the sensor, and the sensor
is placed directly on the dish. Setting the sensor directly on the dish provides consistent standoff distances for each
reading and allows the dish to be aligned with the sensor.
D.8.2.3 Install all connections per the manufacturer’s instructions.
NOTE 1: Erratic readings may be attributed to a fluctuating power supply, such as a cycling hot plate in the
same receptacle. This should be avoided if possible.
Turn the power ON. Once the power switch is turned ON, it takes approximately 15 seconds before the
software boots up and the display comes to life and it takes 15 minutes for the control unit to warm up. To adjust
the control unit settings, the SELECT button is used to cycle the display, and the UP and DOWN buttons are used to
change the settings. An explanation of each item and the required setting is as follows:
1. SIGNAL: This is the initial power-on screen. The display should show a number with the word “signal”
beneath it. If the words “GND SAMPLE” appear, the sample is not properly grounded. For this analysis, since the
evaporating dish is placed on the sensor stand, plugging the sensor stand into the monitor will properly ground the
sample (i.e., the evaporating dish). Refer to the manufacturer’s instructions for making this connection. The signal
is the real-time reading and does not represent the peak. This mode is not used while taking measurements for this
procedure.
2. PEAK: The peak detect mode will search for the maximum OSEE signal and display it. This is the mode
used for taking measurements throughout this procedure. Each reading taken per this manual is a peak reading. The
units on the display are “centi-volts”. Because this unit of measure is not common, the term “counts” will be used,
and is commonly used by the manufacturer.
3. LOW GATE: The low gate setting can be adjusted to indicate when a reading is below established
acceptance criteria. When the reading is below the low gate setting, the display will show the counts and the
message “OUT LOW”. This setting is not required or used in this procedure. Using the UP/DOWN buttons, set the
low gate to 0 count to inactivate it and avoid confusion.
4. HIGH GATE: The high gate setting can be adjusted to indicate when a reading is above established
acceptance criteria. When the reading is above the high gate setting, the display will show the counts and the
message “OUT HIGH”. This setting is not required or used in this procedure. Using the UP/DOWN buttons, set the
high gate to 1000 counts to inactivate it and avoid confusion.
5. GAIN: The gain amplifies the signal, which can be interpreted as a multiplier for the output. There are two
gain settings available, one on the sensor and the other on the control unit.
a. Sensor Gain. On the sensor, the gain setting is indicated by the number (on the outer ring of the rotary
switch) opposite the dot (on the inner ring of the rotary switch). The available settings, from lowest to highest, are
1, 2, 3, 4, 5, 6, 7, 8, 9, and 0. Using the tool provided, set the sensor gain to 4. No further adjustments of the sensor
gain will be made throughout this procedure.
b. Control Unit Gain. On the control unit, the available gain settings are 1, 2, 4, and 8. Using the UP/DOWN
buttons, set the gain to 4. This is a starting point and will be adjusted at the control unit as needed for the
evaporating dish. Each increase in gain will double the output, and each decrease will halve the output.
6. TIME DELAY: This is a standard feature on newer instruments. Time delay is the amount of time that
elapses before a reading is taken (readings are taken in manual mode using ENTER button or automatic mode using
Threshold for Peak as described below). Time delay can be set from 1 to 120 seconds. Using the UP/DOWN
buttons, set the time delay to 1.
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7. THRESHOLD FOR PEAK: It displays the Threshold for Peak setting. Using the UP/DOWN buttons, set
the Threshold for Peak to 1000 counts. The Threshold for Peak automatically triggers a peak search when the signal
is cycled below this value. For instance, suppose that the Threshold for Peak is set at 30 counts, and that an
evaporating dish is measured at 600 counts. When the dish is taken away from the sensor, the signal needs to
decrease below 30 counts to initiate a search for a new reading. As long as it goes below 30 counts, when another
dish is placed under the sensor, the unit will automatically search for a new peak. If it does not drop below 30
counts, a search for a new peak will not be initiated. Using the automatic mode can cause erroneous results for the
use specified in this appendix. This is because the automatic peak search occurs very quickly and the dish or sensor
may not be in place when the peak search is initiated. To force use in the manual mode, the Threshold for Peak is
set at 1000 counts. This will essentially inactivate the automatic feature and a peak search will begin when the
ENTER button is pressed.
8. SAVE CURRENT PARAMETERS: This screen will only be displayed if any of the preceding parameters
were changed. Press the ENTER button to save changes.
D.8.3 Maintenance of SQM. Check the SQM UV lamp intensity, sensor electronics, and control unit
electronics every six months using the following procedure and equipment listed in D.5.1(k), or by sending the
entire unit (control unit and sensor) to the manufacturer. Log all results in data sheets 1 and 2. If the manufacturer
performs the check, obtain the data and log in data sheets 1 and 2. Annotate any corrective action required in the
Remarks column.
D.8.3.1 Sensor electronics.
D.8.3.1.1 Turn the SQM control unit ON. Allow 15 minutes to warm up. Confirm the monitor is in SIGNAL
mode.
D.8.3.1.2 Set the gain settings on the sensor and control unit to the settings used last time acceptance criteria
were established for dishes.
CAUTION 2: When removing the sensor, do not touch the aperture on the end of the sensor. Contamination
can seriously degrade performance.
WARNING 1: Do not look directly into the ultraviolet light source at the end of the sensor because it can cause
eye damage.
D.8.3.1.3 Remove the screws holding the sensor in the stand and remove the sensor.
D.8.3.1.4 Place the Calibration Load (D.5.1(k)) at the end of the sensor. In order to read the calibration load, it
needs to be held steady to yield stable readings. After the reading stabilizes, log the reading in data sheet 1.
D.8.3.1.5 Using the tool provided, increase the sensor gain by one unit from the setting of D.8.3.1.2 and repeat
D.8.3.1.4.
D.8.3.1.6 Using the tool provided, decrease the sensor gain by one unit from the setting of D.8.3.1.2 and repeat
D.8.3.1.4.
D.8.3.1.7 Referring to data sheet 1, for each set of gain settings, compare the first and last reading. If the
reading drops by more than 5 percent, send the entire unit to the manufacturer for servicing. Note the first reading
establishes the acceptance criteria and there is nothing to compare to. Also note that if the gain settings used for
establishing acceptance criteria changed from the last time this calibration was accomplished, there will not be data
to compare to for all of the readings; this is acceptable. When it gets returned from the manufacturer, repeat
D.8.3.1.1 through D.8.3.1.7. This becomes the first reading.
D.8.3.1.8 Restore the gain settings on the sensor and control unit to the settings noted in D.8.3.1.2. Reinstall
the sensor using the screws removed in D.8.3.1.3 and set the sensor per D.8.2.2.
D.8.3.2 UV lamp intensity.
D.8.3.2.1 Turn the SQM control unit ON. Allow 15 minutes to warm up.
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D.8.3.2.2 Connect the detector to the radiometer. The orientation of the electrical connection makes no
difference. Turn the radiometer ON. With the cap installed on the detector for the radiometer, press the ZERO key.
When turned off, batteries retain the zero reading in the memory. If the memory is lost, repeat this step.
D.8.3.2.3 Loosen the screws holding the sensor in the stand so that the sensor can slide relative to the mounting
bracket. Remove the cap from the detector. Place the adapter (D.5.1(k)) on the end of the sensor, and place the
detector beneath the adapter. Slide the sensor down so that everything rests on the stand.
D.8.3.2.4 Press the SIGNAL key on the radiometer to measure the UV light intensity and log in data sheet 2.
Move the detector away from the adapter, then again place it beneath the adapter to take a repeated reading. Take a
total of 10 readings and log in data sheet 2. Add the readings and divide the total by 10 to calculate the average and
log in data sheet 2. A variance in readings of 5 percent is possible because it is difficult to consistently measure
ultraviolet light intensity. As the UV light intensity decreases over time, the light emitted from the surface, and all
of the readings, will drop accordingly. Comparison of the established acceptance criteria for a dish and the UV light
intensity can account for a drop in the established acceptance criteria. Over several years, the gain settings may
need to be adjusted to account for this decrease in readings. The UV light intensity should decrease linearly by a
maximum of 30 percent over a period of 5000 hours. If it exhibits a greater decrease in less hours or exhibits a rapid
drop in UV lamp intensity, contact NAVSEA for direction.
D.8.3.2.5 Turn the radiometer OFF. Replace the cap on the detector. Disconnect the detector from the
radiometer. Tighten the screws holding the sensor and set the sensor per D.8.2.2.
D.8.3.3 Control unit electronics.
D.8.3.3.1 Turn the SQM OFF and unplug the sensor from the rear of the control unit.
NOTE 2: After turning the SQM OFF, it takes about 15 to 30 seconds for it to boot down properly. If it is
turned ON before it is booted down properly, the display will not come on. If this occurs, turn it off, wait about 30
seconds, then turn it on again.
D.8.3.3.2 Wait about 30 seconds, then turn the SQM ON. There will be an error message stating “CONNECT
SENSOR-TURN POWER OFF 1ST”. Press the ENTER key to eliminate this error message. Set the GAIN on the
control unit to 1. Allow 15 minutes to warm up.
D.8.3.3.3 Observe the reading and log in data sheet 2. If the reading is 5 or less, no action is required. If the
reading is more than 5, send the control unit to the manufacturer for adjustment and calibration.
D.8.3.3.4 Restore the gain settings on the control unit to the setting noted in D.10.1.5.
D.8.3.3.5 Turn the SQM OFF and plug the sensor in the rear of the control unit. Wait about 30 seconds, then
turn the SQM ON.
D.8.4 Safety precautions.
D.8.4.1 When handling CFC-113, HCFC-225, or HFE-7100, the safety precautions specified by the material
safety data sheet (MSDS) and 4.4.1.2 shall be followed.
D.8.4.2 When handling Sparkleen, follow the safety precautions specified by the material safety data sheet
(MSDS).
D.8.5 Cleaning of equipment.
D.8.5.1 Rinse the pipet and washing bottle with unused solvent. Clean the beaker with Sparkleen (soaking for
one hour, then agitating by shaking has been shown to be effective), rinse with water several times, and final clean
with unused solvent.
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D.10 Establishing dish acceptance criteria. Each dish has two acceptance criteria: clean dish and 5 ppm (with
or without baseline). The applicable paragraphs and dosing requirements for establishing these acceptance criteria
are summarized in Table D-II. The clean dish and 5 ppm acceptance criteria shall be established for a new dish,
every six months after performing equipment maintenance specified in D.8, and whenever the need is identified
during routine analysis (Section D.11). Normal aging of a dish and the sensor will require periodic determination of
dish acceptance criteria. If baseline applies, the 5 ppm acceptance criteria is required for each batch or lot of
solvent.
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D.10.1 Clean dish acceptance criteria.
NOTE 3: If a dish has been in long-term storage in excess of one year, it may be necessary to remove a thin
corrosion layer. This can be accomplished by applying a small amount of polish with a cotton or foam-tipped swab
and rubbing gently for 1 minute. The recommended polish is available from Buehler, 1-800-283-4537, Buehler
Master Polish Suspension, catalog #40-6375-032.
D.10.1.1 Turn the SQM control unit ON. After 15 seconds when the system boots up, set the mode to PEAK.
Allow 15 minutes to warm up. Check that the control unit gain setting is at 4 for a new dish, or the previous gain
setting recorded on data sheet 3.
D.10.1.2 Using Sparkleen cleaning solution (D.6.2(a)) in a container (D.5.1(i)), THOROUGHLY clean the
evaporating dish by scrubbing by hand using a paper towel (D.5.1(h)) for about one minute. Rinse
THOROUGHLY, for about 20 to 30 seconds, under running tap water. Shake off excess water.
NOTE 4: Do not touch the inside surface after cleaning and do not dry the inside surface with a towel or cloth.
D.10.1.3 Using the washing bottle (D.5.1(d)) filled with CFC-113, HCFC-225, or HFE-7100, tilt the dish and
spray it with solvent to displace the water droplets off of the dish, particularly from the flat area at the bottom of the
evaporating area. Droplets remaining near the top edge are acceptable. The solvent shall be directed into a “solvent
waste” container.
D.10.1.4 Place the dish on a hot plate set per D.8.1.1. Keep the dish on the hot plate until no solvent or water
droplets remain on the surfaces where evaporation occurs. On the flat top edge and bottom, any residual water can
be wiped with a clean cloth.
NOTE 5: Accomplish the following actions as quickly as possible to minimize the time the dish is exposed to
the UV light. Since the monitor is not sensitive to the temperatures specified in this procedure, there is no need to
allow the dish to cool before taking a reading.
D.10.1.5 Slide the dish under the SQM sensor. Place the sensor directly on the top edge of the dish. Align the
dish so that the outside of the dish aligns with the outside of the sensor. Press the ENTER key on the SQM and
observe the reading. Remove the dish. Log the reading on data sheet 3. Place the dish back on the hot plate.
a. If the reading is greater than 1000 counts (off scale), reduce the gain setting on the control unit. Do not
reduce the gain below 2. A gain setting less than 2 indicates a possible problem with the equipment. Check the
equipment by performing D.8.3.
b. If the reading is less than 500 counts, increase the gain setting on the control unit. A gain setting that needs
to be greater than 8 generally indicates a dirty dish or a problem with the equipment. Clean dish per D.10.1.2. If
this does not correct the problem, check the equipment by performing D.8.3.
c. Log the control unit gain setting on data sheet 3.
D.10.1.6 After 3 minutes has elapsed, repeat D.10.1.5 (reading #2).
D.10.1.7 Repeat steps D.10.1.2 to D.10.1.6 (cleaning #2) until two consecutive readings from D.10.1.6, using
the same control unit gain, are within the following acceptable range: the difference between the readings shall be
less than 100 counts.
D.10.1.8 The average of the two acceptable readings shall be recorded in data sheet 3 as the Clean Dish
Acceptance Criteria.
D.10.2 5 ppm acceptance criteria without baseline.
D.10.2.1 Turn the SQM control unit ON. After 15 seconds when the system boots up, set the mode to PEAK.
Allow 15 minutes to warm up. Check that the control unit gain setting is as specified in data sheet 3 for the dish
being used.
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D.10.2.2 Using Sparkleen cleaning solution (D.6.2(a)) in a container (D.5.1(i)), THOROUGHLY clean the
evaporating dish by scrubbing by hand using a paper towel (D.5.1(h)) for about one minute. Rinse
THOROUGHLY, for about 20 to 30 seconds, under running tap water. Shake off excess water.
NOTE 6: Do not touch the inside surface after cleaning and do not dry the inside surface with a towel or cloth.
D.10.2.3 Using the washing bottle (D.5.1(d)) filled with CFC-113, HCFC-225, or HFE-7100, tilt the dish and
spray it with solvent to displace the water droplets off of the dish, particularly from the flat area at the bottom of the
evaporating area. Droplets remaining near the top edge are acceptable. The solvent shall be directed into a “solvent
waste” container.
D.10.2.4 Place the dish on a hot plate set per D.8.1.1. Keep the dish on the hot plate until no solvent or water
droplets remain on the surfaces where evaporation occurs. On the flat top edge and bottom, any residual water can
be wiped with clean cloth.
NOTE 7: Accomplish the following actions as quickly as possible to minimize the time the dish is exposed to
the UV light. Since the monitor is not sensitive to the temperatures specified in this procedure, there is no need to
allow the dish to cool before taking a reading.
D.10.2.5 Slide the dish under the SQM sensor. Place the sensor directly on the top edge of the dish. Align the
dish so that the outside of the dish aligns with the outside of the sensor. Press the ENTER key on the SQM and
observe the reading. Remove the dish. Log the reading on data sheet 3. Place the dish back on the hot plate.
D.10.2.6 After 3 minutes has elapsed, repeat D.10.2.5.
D.10.2.7 Check that the dish baseline cleanliness (reading #2) is within 100 counts of the baseline cleanliness
acceptance criteria recorded in data sheet 3 for the specific dish being used for the analysis. Readings outside this
range indicate a problem with dish cleanliness. Repeat steps D.10.2.2 through D.10.2.6 to check dish cleanliness.
NOTE 8: The solvent used for preparing the laboratory standard needs to be the same as the cleaning solvent
(i.e., if HFE-7100 will be used as the cleaning solvent, then HFE-7100 must be used to prepare the standard).
NOTE 9: Never transfer calibration standard from the laboratory standard to the dish using the pipet to prevent
contamination of the standard.
NOTE 10: If the standard inadvertently reaches the dispenser, the dispenser will contaminate the contents of
the pipet. If this occurs, dump the contents of the pipet into the waste solvent storage flask and fill the pipet several
times above the 0.5 mL mark with unused solvent to clean the pipet.
WARNING 2: Thermal decomposition of solvent can cause harmful vapors. As a check, feel the hot plate with
bare hand to confirm it is only “warm to the touch” prior to evaporating solvent in the dish. If it is hot, determine
the cause and correct the problem before proceeding.
D.10.2.8 For the standard prepared in D.9, if it is used for the first time that day, confirm that the solvent level
is at the last mark on the standard. If it is not, obtain another standard. Shake the standard vigorously for no less
than 15 seconds. Remove the cap from the laboratory standard. Pour approximately 2 to 3 mL of the laboratory
standard into the 10 mL beaker. Immediately replace the cap on the standard to minimize evaporative losses. Fill
the pipet with 0.5 mL of solution by rotating the filler/dispenser knob. With the dish on the hot plate, transfer this
0.5 mL of solution to the evaporating dish by rotating the knob in the opposite direction. Allow the solvent to
completely evaporate.
D.10.2.9 Repeat D.10.2.8 for a total of 3 doses (1.5 mL total) for other than instruments, or 3 doses (1.5 mL
total) for instruments. Clean the beaker and pipet by rinsing with unused solvent.
NOTE 11: Accomplish the following actions as quickly as possible to minimize the time the dish is exposed to
the UV light. Since the monitor is not sensitive to temperatures specified in this procedure, there is no need to allow
the dish to cool before taking a reading.
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D.10.2.10 Slide the dish under the SQM sensor. Place the sensor directly on the top edge of the dish. Align the
dish so that the outside of the dish aligns with the outside of the sensor. Press the ENTER key on the SQM and
observe the reading. Remove the dish. Log the reading in data sheet 3. Place the dish back on the hot plate.
NOTE 12: If an error occurs while taking a reading, such as pressing the wrong key or dropping the dish, the
reading can not be repeated. If this occurs, start over from D.10.2.2.
D.10.2.11 Repeat D.10.2.2 through D.10.2.10 until three data points (they do not have to be consecutive) are
within the following acceptable range.
TABLE D-III. Acceptable range for 5 ppm acceptance criteria without baseline.
Acceptable Range: Maximum allowable difference between
Solvent
highest and lowest reading
CFC-113 60 counts
HCFC-225 50 counts
HFE-7100 30 counts
D.10.2.13 The average of the three acceptable data points shall be recorded in data sheet 3 as the Dish 5 ppm
Acceptance Criteria.
D.10.2.14 At the end of the day or when D.10.2.13 is completed, mark the solvent level on the laboratory
standard.
D.10.3 5 ppm acceptance criteria with baseline.
D.10.3.1 Perform D.10.2 to determine the 5 ppm acceptance criteria for the dish for comparison to baseline.
D.10.3.2 Turn the SQM control unit ON. After 15 seconds when the system boots up, set the mode to PEAK.
Allow 15 minutes to warm up. Check that the control unit gain setting is as specified in data sheet 2 for the dish
being used.
D.10.3.3 Using Sparkleen cleaning solution (D.6.2(a)) in a container (D.5.1(i)), THOROUGHLY clean the
evaporating dish by scrubbing by hand using a paper towel (D.5.1(h)) for about one minute. Rinse
THOROUGHLY, for about 20 to 30 seconds, under running tap water. Shake off excess water.
NOTE 13: Do not touch the inside surface after cleaning and do not dry the inside surface with a towel or cloth.
D.10.3.4 Using the washing bottle (D.5.1(d)) filled with CFC-113, HCFC-225, or HFE-7100, tilt the dish and
spray it with solvent to displace the water droplets off of the dish, particularly from the flat area at the bottom of the
evaporating area. Droplets remaining near the top edge are acceptable. The solvent shall be directed into a “solvent
waste” container.
D.10.3.5 Place the dish on a hot plate set per D.8.1.1. Keep the dish on the hot plate until no solvent or water
droplets remain on the surfaces where evaporation occurs. On the flat top edge and bottom, any residual water can
be wiped with clean cloth.
NOTE 14: Accomplish the following actions as quickly as possible to minimize the time the dish is exposed to
the UV light. Since the monitor is not sensitive to the temperatures specified in this procedure, there is no need to
allow the dish to cool before taking a reading.
D.10.3.6 Slide the dish under the SQM sensor. Place the sensor directly on the top edge of the dish. Align the
dish so that the outside of the dish aligns with the outside of the sensor. Press the ENTER key on the SQM and
observe the reading. Remove the dish. Log the reading on data sheet 3. Place the dish back on the hot plate.
D.10.3.7 After 3 minutes has elapsed, repeat D.10.3.5.
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D.10.3.8 Check that the dish baseline cleanliness (reading #2) is within 100 counts of the baseline cleanliness
acceptance criteria recorded in data sheet 3 for the specific dish being used for the analysis. Readings outside this
range indicate a problem with dish cleanliness. Repeat steps D.10.3.3 through D.10.3.7 to check dish cleanliness.
NOTE 15: The solvent used for preparing the laboratory standard needs to be the same as the cleaning solvent
(i.e., if HFE-7100 will be used as the cleaning solvent, then HFE-7100 must be used to prepare the standard).
NOTE 16: Never transfer calibration standard from the laboratory standard to the dish using the pipet to
prevent contamination of the standard.
NOTE 17: If the standard inadvertently reaches the dispenser, the dispenser will contaminate the contents of
the pipet. If this occurs, dump the contents of the pipet into the waste solvent storage flask and fill the pipet several
times above the 0.5 mL mark with unused solvent to clean the pipet.
WARNING 3: Thermal decomposition of solvent can cause harmful vapors. As a check, feel the hot plate with
bare hand to confirm it is only “warm to the touch” prior to evaporating solvent in the dish. If it is hot, determine
the cause and correct the problem before proceeding.
D.10.3.9 Transfer 2 to 3 mL of unused solvent into the 10 mL beaker. Fill the pipet with 0.5 mL of solution by
rotating the filler/dispenser knob. With the dish on the hot plate, transfer this 0.5 mL of solution to the evaporating
dish by rotating the knob in the opposite direction. Allow the solvent to completely evaporate. Repeat for a total of
2 doses.
NOTE 18: Accomplish the following actions quickly as possible to minimize the time the dish is exposed to the
UV light. Since the monitor is not sensitive to temperatures specified in this procedure, there is no need to allow the
dish to cool before taking a reading.
D.10.3.10 Slide the dish under the SQM sensor. Place the sensor directly on the top edge of the dish. Align the
dish so that the outside of the dish aligns with the outside of the sensor. Press the ENTER key on the SQM and
observe the reading. Remove the dish. Log the reading in data sheet 3. Place the dish back on the hot plate.
NOTE 19: If an error occurs while taking a reading, such as pressing the wrong key or dropping the dish, the
reading can not be repeated. If this occurs, start over from D.10.3.3.
D.10.3.11 Compare to the data taken in D.10.3.1. If the reading is greater than or equal to the Dish 5 ppm
Acceptance Criteria, then the baseline solvent is acceptable for use. Continue with dosing the dish with 5 ppm
standard as specified in the following paragraphs. If the reading is less than the Dish 5 ppm Acceptance Criteria,
perform troubleshooting to determine the source of the contamination.
D.10.3.12 For the standard prepared in D.9, if it is used for the first time that day, confirm that the solvent level
is at the last mark on the standard. If it is not, obtain another standard. Shake the standard vigorously for no less
than 15 seconds. Remove the cap from the laboratory standard. Pour approximately 2 to 3 mL of the laboratory
standard into the 10 mL beaker. Immediately replace the cap on the standard to minimize evaporative losses. Fill
the pipet with 0.5 mL of solution by rotating the filler/dispenser knob. With the dish on the hot plate, transfer this
0.5 mL of solution to the evaporating dish by rotating the knob in the opposite direction. Allow the solvent to
completely evaporate.
D.10.3.13 Repeat D.10.3.12 for a total of 3 doses (1.5 mL total). Clean the beaker and pipet by rinsing with
unused solvent.
NOTE 20: Accomplish the following actions as quickly as possible to minimize the time the dish is exposed to
the UV light. Since the monitor is not sensitive to temperatures specified in this procedure, there is no need to allow
the dish to cool before taking a reading.
D.10.3.14 Slide the dish under the SQM sensor. Place the sensor directly on the top edge of the dish. Align the
dish so that the outside of the dish aligns with the outside of the sensor. Press the ENTER key on the SQM and
observe the reading. Remove the dish. Log the reading in data sheet 3. Place the dish back on the hot plate.
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MIL-STD-1330D(SH)
APPENDIX D
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NOTE 21: If an error occurs while taking a reading, such as pressing the wrong key or dropping the dish, the
reading can not be repeated. If this occurs, start over from D.10.3.3.
D.10.3.15 Repeat D.10.3.3 through D.10.3.14 until three data points (they do not have to be consecutive) are
within the following acceptable range.
TABLE D-IV. Acceptable range for 5 ppm acceptance criteria with baseline.
Acceptable Range: Maximum allowable difference between
Solvent
highest and lowest reading
CFC-113 60 counts
HCFC-225 50 counts
HFE-7100 30 counts
D.10.3.16 The average of the three acceptable data points shall be recorded in data sheet 3 as the Dish 5 ppm
Acceptance Criteria with Baseline.
D.10.3.17 At the end of the day or when D.10.3.16 is completed, mark the solvent level on the laboratory
standard.
D.11 Procedure for performing analysis. For instrument cleaning, the sample is taken in conjunction with
performing the analysis as specified in D.7. For other than instrument cleaning, the sample is taken in a container
during the cleaning process. Log all results in data sheet 4. Results shall be retained as long as the item cleaned is
in use.
D.11.1 Assign a unique control number for the analysis and log in data sheet 4.
D.11.2 Turn the SQM control unit ON. After 15 seconds when the system boots up, set the mode to PEAK.
Allow 15 minutes to warm up. Check that the control unit gain setting is as specified in data sheet 3 for the dish that
will be used for the analysis.
D.11.3 Using Sparkleen cleaning solution (D.6.2(a)) in a container (D.5.1(i)), THOROUGHLY clean the
evaporating dish by scrubbing by hand using a paper towel (D.5.1(h)) for about one minute. Rinse
THOROUGHLY, for about 20 to 30 seconds, under running tap water. Shake off excess water.
NOTE 22: Do not touch the inside surface after cleaning and do not dry the inside surface with a towel or cloth.
D.11.4 Using the washing bottle (D.5.1(d)) filled with CFC-113, HCFC-225, or HFE-7100, tilt the dish and
spray it with solvent to displace the water droplets off of the dish, particularly from the flat area at the bottom of the
evaporating area. Droplets remaining near the top edge are acceptable. The solvent shall be directed into a “solvent
waste” container.
WARNING 4: Thermal decomposition of solvent can cause harmful vapors. As a check, feel the hot plate with
bare hand to confirm it is “warm to the touch” prior to evaporating solvent in the dish. If it appears too warm,
determine the cause and take the necessary corrective action.
D.11.5 Place the dish on a hot plate set per D.8.1.1. Keep the dish on the hot plate until no solvent or water
droplets remain on the surfaces where evaporation occurs. On the flat top edge and bottom, any residual water can
be wiped with a clean cloth.
NOTE 23: Accomplish the following actions as quickly as possible to minimize the time the dish is exposed to
the UV light. Since the monitor is not sensitive to the temperatures specified in this procedure, there is no need to
allow the dish to cool before taking a reading.
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MIL-STD-1330D(SH)
APPENDIX D
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D.11.6 Slide the dish under the SQM sensor. Place the sensor directly on the top edge of the dish. Align the
dish so that the outside of the dish aligns with the outside of the sensor. Press the ENTER key on the SQM and
observe the reading. Remove the dish. Log the reading on data sheet 4. Place the dish back on the hot plate.
a. The above actions shall be accomplished as quickly as possible to minimize the time the dish is exposed to
the UV light.
b. Since the monitor is not sensitive to the temperatures specified in this procedure, there is no need to allow
the dish to cool before taking a reading.
D.11.7 After 3 minutes has elapsed, repeat D.11.6.
D.11.8 Check that the dish cleanliness (reading #2) is within 100 counts of the Clean Dish Acceptance Criteria
recorded in data sheet 3 for the specific dish being used for the analysis. Readings outside this range indicate either
a problem with dish cleanliness or equipment operation. Repeat D.11.3 through D.11.7 to check dish cleanliness. If
still unable to meet the baseline cleanliness acceptance criteria, perform equipment maintenance per D.8 and
determine new dish acceptance criteria as specified in D.10.
D.11.9 Shake the sample container vigorously for no less than 15 seconds. Remove the cap from the sample
container. Pour approximately 2 to 3 mL of the sample into the 10 mL beaker. Immediately replace the cap on the
sample to minimize evaporative losses. Fill the pipet with 0.5 mL of solution by rotating the filler/dispenser knob.
With the dish on the hot plate, transfer this 0.5 mL of solution to the evaporating dish by rotating the knob in the
opposite direction. Allow the solvent to evaporate. Repeat for a total of 2 doses.
D.11.10 Slide the dish under the SQM sensor. Place the sensor directly on the top edge of the dish. Align the
dish so that the outside of the dish aligns with the outside of the sensor. Press the ENTER key on the SQM and
observe the reading. Remove the dish. Log the reading in data sheet 4. Place the dish back on the hot plate.
a. The above actions shall be accomplished as quickly as possible to minimize the time the dish is exposed to
the UV light.
b. Since the monitor is not sensitive to temperatures specified in this procedure, there is no need to allow the
dish to cool before taking a reading.
c. If an error occurs while taking a reading, such as pressing the wrong key or dropping the dish, the reading
cannot be repeated. If this occurs, start over from D.11.3.
NOTE 24: Oil and grease, along with most other contaminants, will cause the counts to decrease. In rare
instances, such as some surfactants, the counts can increase.
D.11.11 Compare the reading from D.11.10 to the Clean Dish Acceptance Criteria and the Dish 5 ppm
Acceptance Criteria recorded in data sheet 3 as described below, and as shown in Table D-V and Figure 5:
a. If the reading is less than the Clean Dish Acceptance Criteria plus 50 counts and greater than or equal to
the Dish 5 ppm Acceptance Criteria, the results are acceptable and are reported as less than 5 ppm oil and grease.
Log all results on data sheet 4.
b. If the reading is less than the Dish 5 ppm Acceptance Criteria, the results are not acceptable and the
instrument requires recleaning.
c. If the reading is greater than or equal to the Clean Dish Acceptance Criteria plus 50 counts, the results are
not acceptable and the instrument requires recleaning.
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MIL-STD-1330D(SH)
APPENDIX D
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MIL-STD-1330D(SH)
APPENDIX D
w/ Change 1
DATA SHEET 1. Surface Quality Monitor maintenance record for sensor electronics.
Sensor Gain Setting used for Increase Sensor Gain Setting Decrease Sensor Gain
establishing dish acceptance by 1 unit (e.g., 5) Setting by 1 unit (e.g., 3)
criteria from D.S. 3 (e.g., 4) Setting:_________ Setting:_________
Setting:_________ (see D.8.3.1.5) (see D.8.3.1.6)
Name and
Date (see D.8.3.1.2)
ID
Acceptance Acceptance Acceptance
SQM Criteria = SQM Criteria = SQM Criteria =
Reading SQM reading Reading SQM reading Reading SQM reading
X 0.95 X 0.95 X 0.95
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MIL-STD-1330D(SH)
APPENDIX D
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DATA SHEET 2. Surface Quality Monitor maintenance record for lamp intensity and control unit electronics.
Control Unit Electronics-
Lamp Intensity
Date Reading Name and ID SQM Reading 1/ Remarks
(see D.8.3.2.4)
(see D.8.3.3.3)
1
2
3
Average
1
2
3
Average
1
2
3
Average
1
2
3
Average
1
2
3
Average
NOTE:
1/
If the reading is more than 5, send the control unit to the manufacturer for adjustment and calibration.
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MIL-STD-1330D(SH)
APPENDIX D
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Solvent used for standard:____________(Shall be same as solvent used for cleaning the instrument.)
Reading #2
SQM readings
Reading/Dose and average
Trial 1 Trial 2 Trial 3
Cleaned Dish
Reading #1
Reading #2 2/
Dish 5 ppm Acceptance Criteria
Dose #3
Average Dose #3 3/
(Dish 5 ppm Acceptance Criteria)
NOTES:
2/
For all trials, for reading #2, the difference between the clean dish acceptance criteria and each result must be
less than 100 counts.
3/
For dose #3, calculate the difference between the highest and lowest readings. If it meets the acceptance
criteria in Table D-III or D-IV, as applicable, the data is acceptable. If it does not meet the acceptance criteria,
perform additional trials until results are acceptable.
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MIL-STD-1330D(SH)
APPENDIX D
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Control Number:____________________
_____________________________________________________________________________________________
Evaporating Dish:__________________
Cleaned Dish
Reading #1
Reading #2 1/
Dose #3 2/
NOTES:
1/
Reading #2 must be within 100 counts of Clean Dish Cleanliness
Acceptance Criteria entered above from data sheet 3.
2/
(a) If dose #3 is less than the Clean Dish Acceptance Criteria plus 50
counts and greater than or equal to the Dish 5 ppm Acceptance Criteria,
the results are acceptable and are reported as less than 5 ppm oil and
grease.
(b) If dose #3 is less than the Dish 5 ppm Acceptance Criteria, the results
are not acceptable and the item requires recleaning.
(c) If dose #3 is greater than or equal to the Clean Dish Acceptance
Criteria plus 50 counts, the results are not acceptable and the item requires
recleaning.
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MIL-STD-1330D(SH)
APPENDIX D
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Remarks:________________________________________________________________________________
________________________________________________________________________________________
________________________________________________________________________________________.
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MIL-STD-1330D(SH)
APPENDIX E
w/ Change 1
NAVSEA APPROVED HALOGENATED SOLVENTS
E.1 SCOPE
E.1.1 Scope. This appendix is a mandatory part of the standard. The information contained herein is intended
for compliance. This appendix identifies the NAVSEA approved halogenated solvents, and specifies information
regarding safe and effective use.
E.2 APPLICABLE DOCUMENTS
E.2.1 General. The documents listed in this section are specified in Appendix E of this standard. This section
does not include documents cited in other sections of this standard or recommended for additional information or as
examples. While every effort has been made to ensure the completeness of this list, document users are cautioned
that they must meet all specified requirements of documents cited in Appendix E of this standard, whether or not
they are listed.
E.2.2 Government documents.
E.2.2.1 Specifications, standards, and handbooks. The following specifications, standards, and handbooks
form a part of this document to the extent specified herein. Unless otherwise specified, the issues of these
documents are those cited in the solicitation or contract.
COMMERCIAL ITEM DESCRIPTIONS
A-A-50427 - Cleaning Compound, Solvent, 1,1-Dichloro-1- Fluoroethane, HCFC-
141B, for Oxygen Systems
A-A-59150 - Cleaning Compound, Solvent, Hydrofluoroether (HFE)
A-A-59743 - Cleaning Compound Solvent, Dichloropentafluoropropane (HCFC-225)
DEPARTMENT OF DEFENSE SPECIFICATIONS
MIL-C-81302 - Cleaning, Compound, Solvent, Trichlorotrifluoroethane
(Copies of these documents are available online at http://assist.daps.dla.mil/quicksearch/ or
http://assist.daps.dla.mil or from the Standardization Document Order Desk, 700 Robbins Avenue, Building 4D,
Philadelphia, PA 19111-5094.)
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MIL-STD-1330D(SH)
APPENDIX E
w/ Change 1
TABLE E-I. NAVSEA approved halogenated solvents. Continued.
Approved halogenated solvents 1/
Attribute
CFC-113 2/ HCFC-141b 3/ HCFC-225 4/ HFE-7100 5/
Ozone depleting substance Yes Yes Yes No
Ozone depletion potential 0.8 0.11 0.03 0.0
Production phase-out 1996 2003 2015 NA
Process verification methods
1. PTFE (Teflon) C C C C
2. PCTFE (Kel-F) C C C C
3. Vespel SP-21 C C C C
4. Viton 12L 1L 1L 1L
5. Silicone I 12L I I
NOTES:
1/
HFE-7100 is the preferred solvent for cleaning gages and instruments. HCFC-225 is the preferred solvent for
cleaning oxygen-nitrogen producers.
2/
For naval activities, the use of CFC-113 is restricted to those authorized by NAVSEA to access the mission
critical reserve maintained by the Defense Logistics Agency or reserves maintained by Naval Shipyards.
Refer to Navy ODS Advisories 95-01 and 96-01 for additional information. CFC-113 procured for gauge
cleaning shall be equivalent to MIL-C-81302, Type I. CFC-113 procured for oxygen-nitrogen producer
cleaning and field wipe shall be equivalent to MIL-C-81302, Type I or II. Recycled CFC-113 shall be
equivalent to MIL-C-81302, Type I, with the following exceptions: moisture content shall be 35 ppm
maximum; organic cleanliness shall be less than 5 ppm determined as specified in 5.13.2; and particulate
cleanliness shall be as specified in 5.13.3.2.
3/
Domestic availability of HCFC-141b is extremely limited based on the production phase-out, and there is no
mission critical reserve. If available, HCFC-141b in accordance with A-A-50427 can be used for cleaning
gauges and oxygen-nitrogen producers. To comply with environmental regulations, and since approved
alternatives exist, HCFC-141b should not be used for field wipe. Be advised that HCFC-141b is reported to
have upper and lower explosion limits of 17.7 and 7.6 percent, respectively. When purging or drying
equipment cleaned with HCFC-141b, ensure purging is performed with nitrogen and is directed to a well
ventilated area free of any ignition sources. Recognize that HCFC-141b at the lower explosive level is toxic
representing an immediate hazard to life. HCFC-141b in accordance with A-A-50427 has been satisfactory
tested for compatibility with gaseous and liquid oxygen demonstrating no ignition or flash point.
4/
HCFC-225 in accordance with A-A-59743 has been satisfactory tested for compatibility with gaseous and
liquid oxygen demonstrating no ignition or flash points, and is available as either HCFC-225G or HCFC-
225M. The recommended 8-hour time weighted average exposure for HCFC-225G is 400 ppm and for
HCFC-225M is 100 ppm. The recommended short term (30-minute) exposure limit for HCFC-225G is 900
ppm and for HCFC-225M is 180 ppm. HCFC-225G in accordance with A-A-59743 is approved for cleaning
gauges, oxygen-nitrogen producers and for field wipe. HCFC-225M in accordance with A-A-59743 is
approved for oxygen-nitrogen producers when appropriate ventilation and other engineering controls can
minimize personnel exposure. HCFC-225M in accordance with A-A-59743 should not be used shipboard, for
gauges or for field wipe because of the low allowable exposure limit.
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MIL-STD-1330D(SH)
APPENDIX E
w/ Change 1
TABLE E-I. NAVSEA approved halogenated solvents. Continued.
NOTES:
5/
HFE-7100 in accordance with A-A-59150 is approved for use to clean gages and instruments. Since HFE-
7100 has marginal hydrocarbon soil removal performance, it shall not be used as a precleaner. An acceptable
precleaner is HFE-71DE, which is a blend of HFE-7100 and 1,2 TransDichloroethylene (TDCE). This solvent
has soil removal performance similar to CFC-113. However, HFE-71DE is not compatible with gaseous or
liquid oxygen, and is more toxic than CFC-113, having a vendor recommended allowable exposure limit of
200 ppm. Therefore, HFE-71DE shall only be used as a precleaner. The performance of HFE-7100 as a wipe
solvent is dependent on the type of soil being removed. HFE-7100 is an excellent wipe solvent for
halogenated oils and greases. HFE-7100 is a poor solvent for hydrocarbon oils and greases including silicone.
6/
For critical applications, a NAVSEA approved halogenated solvent may only be used for field wipe with local
engineering approval.
7/
The only non-metallic materials listed are those common to oxygen systems. For other materials, consult the
manufacturer, local engineering, or NAVSEA. Where specific information is lacking, perform compatibility
testing as specified in A.3.1 of Appendix A.
8/
C = Compatible. 12L = Limit exposure to a maximum of 12 hours per cleaning. 1L = Limit exposure to a
maximum of 1 hour per cleaning. I = Incompatible. NT = Not tested.
Preparing activity:
Navy – SH
(Project 4730-2352-000)
NOTE: The activities listed above were interested in this document as of the date of this document. Since
organizations and responsibilities can change, you should verify the currency of the information above using the
ASSIST Online database at http://assist.daps.dla.mil.
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