1、 DETAIL SPECIFICATION SPECTROMETRIC OIL STANDARDS This specification is approved for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 Scope. This specification covers the requirements for blended spectrometric oil standards for use in calibrating or verifying the calibr
2、ation of spectrometers used in spectrometric analysis of metallic elements found in oils and other fluids. 1.2 Classification. The blended spectrometric oil standards are of the following types: Type Description of the Spectrometric Oil Standards Type D19-0 Spectrometric oil standards (SOS) with 0 e
3、lements D19-XXX1 Series of Spectrometric oil standards (SOS) with 19 elements (Aluminum, Chromium, Copper, Iron, Lead, Magnesium, Nickel, Silicon, Silver, Sodium, Tin, Titanium, Boron, Molybdenum, Zinc, Barium, Cadmium, Manganese, Vanadium). D12-XXX1 Spectrometric oil standards (SOS) with 12 element
4、s (Aluminum, Chromium, Copper, Iron, Lead, Magnesium, Nickel, Silicon, Silver, Sodium, Tin, Titanium) D3-100 Spectrometric oil standards (SOS) with 3 elements (Boron, Molybdenum, Zinc) D21-XXX1 Spectrometric oil standards (SOS) with 21 elements (Aluminum, Chromium, Copper, Iron, Lead, Magnesium, Nic
5、kel, Silicon, Silver, Sodium, Tin, Titanium, Boron, Molybdenum, Zinc, Barium, Cadmium, Manganese, Vanadium, Calcium, Phosphorus) Note: 1 The “XXX” is replaced by the corresponding concentration of the elements in the applicable standard. For example D19-005 contains 5 parts per million (ppm) of the
6、19 elements listed in the description. The D19 and D21 series of standards are produced in the nominal concentrations of 5, 10, 30, 50, 80, 100, 120, 300, 500, 700, and 900 ppm. The D12 series of standards are produced in the nominal concentrations of 5, 10, 30, 50, 100, and 300 ppm. AMSC N/A FSC 91
7、50 Comments, suggestions, or questions on this document should be addressed to: Commander, Naval Air Warfare Center, Aircraft Division, Code 4L8000B120-3, Highway 547, Lakehurst, NJ 08733-5100 or emailed to michael.sikoranavy.mil. Since contact information can change, you may want to verify the curr
8、ency of this address information using the ASSIST Online database at https:/assist.dla.mil. METRIC MIL-DTL-85694A 12 August 2013 DoD-S-85694 20 October 1986Reinstated after 12 August 2013 and may be used for new and existing designs and acquisitions. Provided by IHSNot for ResaleNo reproduction or n
9、etworking permitted without license from IHS-,-,-MIL-DTL-85694A 2 2. APPLICABLE DOCUMENTS 2.1 General. The documents listed in this section are specified in sections 3 and 4 of this specification. This section does not include documents cited in other sections of this specification or recommended fo
10、r 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 cited in sections 3 and 4 of this specification, whether or not they are listed. 2.2 Non-Government publicati
11、ons. The following documents 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. ASTM INTERNATIONAL ASTM D92 - Standard Test Method for Flash and Fire Points by Cleveland Open Cup Test
12、er ASTM D97 - Standard Test Method for Pour Point of Petroleum Products ASTM D445 - Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity) ASTM D2270 - Standard Practice for Calculating Viscosity Index from Kinematic Viscosity at 40 and
13、100 C ASTM D2273 - Standard Test Method for Trace Sediment in Lubricating Oils ASTM D4052 - Standard Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density Meter ASTM D4057 - Standard Practice for Manual Sampling of Petroleum and Petroleum Products ASTM D4177 - Stan
14、dard Practice for Automatic Sampling of Petroleum and Petroleum Products ASTM D5185 - Standard Test Method for Determination of Additive Elements, Wear Metals, and Contaminants in Used Lubricating Oils and Determination of Selected Elements in Base Oils by Inductively Coupled Plasma Atomic Emission
15、Spectrometry ASTM D6595 - Standard Test Method for Determination of Wear Metals and Contaminants in Used Lubricating Oils or Used Hydraulic Fluids by Rotating Disc Electrode Atomic Emission Spectrometry (Copies of these documents are available online at www.astm.org or from ASTM International, 100 B
16、arr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959.) AMERICAN SOCIETY FOR QUALITY (ASQ) ASQ-Z1.4 - Sampling Procedures and Tables for Inspection by Attributes. (Copies of this document are available online at www.asq.org or from the American Society for Quality, P.O. Box 3005, 611 East
17、Wisconsin Avenue, Milwaukee, WI 53201-4606.) Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-85694A 3 SAE INTERNATIONAL SAE J1966 Lubricating Oils, Aircraft Piston Engine (Non-Dispersant Mineral Oil) (Copies of this document are available fro
18、m http:/www.sae.org or from the SAE International, 400 Commonwealth Drive, Warrendale, PA 15096-0001.) 2.3 Order of precedence. Unless otherwise noted herein or in the contract, in the event of a conflict between the text of this document and the references cited herein, the text of this document ta
19、kes precedence. Nothing in this document, however, supersedes applicable laws and regulations unless a specific exemption has been obtained. 3. REQUIREMENTS 3.1 Qualification. The spectrometric oil standards furnished under this specification shall be products that are authorized by the qualifying a
20、ctivity for listing on the applicable qualified products list before contract award (see 4.2 and 6.3). 3.2 Material. The standards shall be prepared from metallo-organic concentrates and base oil. 3.2.1 Metallo-organic concentrates. The metallo-organic concentrates shall consist of metallo-organic o
21、r organic oil-miscible liquid compounds or solutions and a fully compatible preservative, stabilizing additive. The compounds shall be fully soluble/miscible in the base oil. 3.2.2 Base oil. The base oil for blending the standards shall be an SAE 50 mineral oil that meets the requirements of Table I
22、, which is analogous to an SAE J1966 non-additive mineral aircraft engine lubricating oil. The base oil shall be tested to verify that no trace metals exceed 1 part per million (ppm), milligrams per kilogram. 3.3 Spectrometric oil standards (SOS). The spectrometric oil standards shall be prepared us
23、ing materials specified in 3.2 to the concentration specified in the contract. Nominal concentrations are 5 ppm, 10 ppm, 30 ppm, 50 ppm, 80 ppm, 100 ppm, 120 ppm, 300 ppm, 500 ppm 700 ppm, and 900 ppm for types D19-XXX and D21-XXX; 5 ppm, 10 ppm, 30 ppm, 50 ppm, 100 ppm, and 300 ppm for type D12-XXX
24、; 100 ppm for type D3-100; 0 ppm for type D19-0. 3.3.1 Type D19-0. Type D19-0 shall be a 0 standard that meets the requirements specified in Table I and does not exceed the elemental requirements in Table II. 3.3.2 Type D19-XXX. Type D19-XXX spectrometric oil standard (SOS) shall meet the requiremen
25、ts specified in Table I and contain the elements at the appropriate concentrations as listed for Type D19 standards in Table II. Nominal concentrations for D19 standards are 5 ppm, Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-85694A 4 10 p
26、pm, 30 ppm, 50 ppm, 80 ppm, 100 ppm, 120 ppm, 300 ppm, 500 ppm, 700 ppm, and 900 ppm. 3.3.3 Type D12-XXX. Type D12-XXX spectrometric oil standard (SOS) shall meet the requirements specified in Table I and contain the elements at the appropriate concentrations as listed for Type D12 standards in Tabl
27、e II. Nominal concentrations for D19 standards are 5 ppm, 10 ppm, 30 ppm, 50 ppm, 100 ppm, and 300 ppm. 3.3.4 Type D3-100. Type D3-100 spectrometric oil standard (SOS) shall meet the requirements specified in Table I and contain the elements at the concentration of 100 ppm as listed for Type D3 stan
28、dards in Table II. 3.3.5 Type D21-XXX. Type D21-XXX spectrometric oil standard (SOS) shall meet the requirements specified in Table I and contain the elements at the appropriate concentrations as listed for Type D21 in Table II. Nominal concentrations for D21 standards are 5 ppm, 10 ppm, 30 ppm, 50
29、ppm, 80 ppm, 100 ppm, 120 ppm, 300 ppm, 500 ppm, 700 ppm, and 900 ppm. 3.4 Homogeneity. All blended spectrometric oil standards shall be homogeneous, free of sediment or precipitate and shall not indicate any mirroring or silvering appearance from the silver element. 3.5 Spectrometric oil standards
30、stability. The spectrometric oil standards shall have a shelf life stability of not less than 30 months for Types D12-XXX and D19-0 and not less than 12 months for Types D19-XXX, D21-XXX, and D3-100. Shelf life beyond the above limits shall be established on laboratory test data (see 6.3). 3.6 Toxic
31、ity. The spectrometric oil standards shall have no adverse effect on the health of personnel when used for its intended purpose in accordance with the safety standards issued by the Occupational Safety and Health Administration (OSHA) (see 6.5 and 6.6). 3.7 Properties. Spectrometric oil standards sh
32、all meet all of the requirements of this specification when tested as specified in Table I and 4.4.1 through 4.4.2. 3.8 Unit pack. Spectrometric oil standards shall meet all of the unit pack requirements of this specification as specified in 3.8.1 through 3.8.3. 3.8.1 Containers. Natural high-densit
33、y polyethylene cylinder bottles with 24/410 neck finish, 8 ounce capacity, shall be used. The bottles shall have a 24/410 white polypropylene unlined flip top cap and a 24/410 natural unlined low-density polyethylene Yorker cap with red tip. 3.8.2 Packing. The natural high-density polyethylene cylin
34、der bottles shall be packed in Kraft mailing tubes with end caps (2.5 x 7 x 0.060). Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-85694A 5 3.8.3 Labeling. All containers and mailing tubes shall be labeled in accordance with the applicable f
35、ederal, state, and municipal laws, statutes, regulations, and ordinances. In addition to the labeling, the following shall appear on each container. Shelf Life/Expiration Date National Stock Number (NSN) “Keep closed when not in use” “Store at 50-80 F” “Protect from bright light, humidity, and water
36、” TABLE I. Chemical and physical property requirements and test methods. Physical property Requirement Test Method Density at 60 F report ASTM D4052 Viscosity (mm2/s at 100 C) 16.3 min., 21.9 max. ASTM D445 Viscosity Index, Min 85 ASTM D2270 Trace Sediment 0.005 ml/100 mL Oil max. ASTM D2273 Pour po
37、int -12 C max. ASTM D97 Flash point, minimum (COC) 243 C ASTM D92 Metal Elements (Rotrode-AES) See Table IV ASTM D6595 Metal Elements (ICP-AES) See Table V ASTM D5185 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-85694A 6 TABLE II. List of
38、elements and formulations by type. Element (chemical symbol) Spectrometric Oil Standards Types D19-0 D21-XXX D19-XXX D12-XXX D3-100 Aluminum (Al) 1 ppm 1.00 X 1.00 X 1.00 X Chromium (Cr) 1 ppm 1.00 X 1.00 X 1.00 X Copper (Cu) 1 ppm 1.00 X 1.00 X 1.00 X Iron (Fe) 1 ppm 1.00 X 1.00 X 1.00 X Lead (Pb)
39、1 ppm 1.00 X 1.00 X 1.00 X Magnesium (Mg) 1 ppm 1.00 X 1.00 X 1.00 X Nickel (Ni) 1 ppm 1.00 X 1.00 X 1.00 X Silicon (Si) 1 ppm 1.00 X 1.00 X 1.00 X Silver (Ag) 1 ppm 1.00 X 1.00 X 1.00 X Sodium (Na) 1 ppm 1.00 X 1.00 X 1.00 X Tin (Sn) 1 ppm 1.00 X 1.00 X 1.00 X Titanium (Ti) 1 ppm 1.00 X 1.00 X 0.92
40、 X Boron (B) 1 ppm 1.00 X 1.00 X 1.15 X Molybdenum (Mo) 1 ppm 1.00 X 1.00 X 0.85 X Zinc (Zn) 1 ppm 1.00 X 1.00 X 1.00 X Barium (Ba) 1 ppm 1.00 X 1.00 X Cadmium (Cd) 1 ppm 1.00 X 1.00 X Manganese (Mn) 1 ppm 1.00 X 1.00 X Vanadium (V) 1 ppm 1.00 X 1.00 X Calcium (Ca) 1 ppm 1.00 X Phosphorus (P) 1 ppm
41、1.00 X Where X = nominal concentration of spectrometric oil standard in ppm 4. VERIFICATION 4.1 Classification of inspections. The inspection requirements specified herein are classified as follows: a. Qualification inspection (see 4.2). b. Conformance inspection (see 4.3). 4.2 Qualification inspect
42、ion. Qualification inspection shall consist of testing to all the tests specified in Table I and 4.4 through 4.4.3. The extended storage stability test (see 4.4.3) shall be performed after the candidate product has passed all other qualification tests. Tentative qualification approval may be granted
43、 to products undergoing the extended storage stability tests. Upon successful completion of the extended storage stability test, full qualification approval may be granted. Failure to pass the extended storage stability test is cause for withdrawal of qualification approval. Provided by IHSNot for R
44、esaleNo reproduction or networking permitted without license from IHS-,-,-MIL-DTL-85694A 7 4.2.1 Requalification. Requalification shall be required when any reformulation or change is made in the source of manufacture, purity, or composition of the base oil or organo-metallic concentrates. A minor c
45、hange in the oil formulation may be made without requalification testing, but only after notification to, and approval by, the qualification activity (see 6.3). 4.2.2 Sampling. Qualification samples shall consist of six 8 ounce bottles of each type D21-XXX and D19-XXX in nominal concentrations of 5
46、ppm, 10 ppm, 30 ppm, 50 ppm, 80 ppm, 100 ppm, 120 ppm, 300 ppm, 500 ppm, 700 ppm, and 900 ppm; six 8 ounce bottles of type D12-XXX in nominal concentrations of 5 ppm, 10 ppm, 30 ppm, 50 ppm, 100 ppm, and 300 ppm; six bottles of Type D3-100 and six bottles of Type D19-0 (see 6.3.1 and 6.3.2). 4.3 Con
47、formance inspection. Conformance inspection shall consist of the tests specified in Table III. Failure to pass any conformance test shall be cause for rejection. TABLE III. Conformance tests. Physical property Requirement Test Method Viscosity (mm2/s at 100 C) 16.3 min., 21.9 max. ASTM D445 Metal El
48、ements (ICP-AES) See Table V ASTM D5185 4.3.1 Sampling and inspection. Each bulk lot (see 6.4) of material for conformance inspection shall be sampled at random in accordance with ASTM D4057 or ASTM D4177. A sample of two 8 ounce bottles of every production lot supplied to the procuring activity sha
49、ll be forwarded to the Naval Air Station Receiving Officer, HAZMART Bldg. 2385, Sample (AIR-4.4.6.1), 22680 Hammond Road, Patuxent River, MD 20670. 4.3.2 Examination of filled containers. A random sample of filled containers from each lot (see 6.4), taken in accordance with ASQ-Z1.4 shall be examined with regard to fill, closure, sealing and leakage. Reject any container having one or more def
