1、.- - - MIL-V-13750B AO 9997706 0498063 A -= I - - _- MI L-V-l3750B(MR) 18 February 1972 SUPERSEDING MI L-V-l3750A(MR) 9 February 1966 MILITARY SPECIFICATION VARNISH, PHENOL-FORMALDEHYDE, CLEAR AND ALUMINUM PIGMENTED 1. SCOPE 1.1 Scope, This specification covers two grades and four types of clear It
2、also provides for two compo- and aluminum pigmented para-phenyl phenol-formaldehyde resin air drying varnishes for use on amnunition (see 6.1). sitions one of which is suitable for use under AIR POLLUTION REGULATIONS (see 6.4). 1.2 Classification. 1.2.1 Grades. The varnishes (clear and aluminized) c
3、overed by this speci- fication shall be furnished in the following grades as specified. Grade A - Tung oil para-phenyl phenol-forma Grade B - Linseed oil para-phenyl phenol-fo 1.2.2 Types. Grade A and B varnishes shall be listed in Table I. dehyde res i n va rn i sh . maldehyde resin varnish. furnis
4、hed in the four types 1.2.3 Compsitins. The varnishes covered by this specification shall be of the following compositions as specified. Composition G - General use. Composition L - Limited use (see 6.4). Licensed by Information Handling ServicesLicensed by Information Handling ServicesMIL-V-L3750B
5、0 W 9777706 047Ob5 L = MI L-V- 137506 (MR) 3.2.1 Composition L. The vehicle shall be the same as 3.2 except the volatile solvents used shall conform to the follow ments by volume when tested as in 4.4.3. and Tab e I ng requ re- (a) (b) Ethyl benzene and toluene: 20 percent maximum. (c) (d) Ketones:
6、negative. (e) Total of a + b: 20 percent maximum. Aromatic compounds with eight or more carbon atoms except ethyl benzene: 8 percent maximum. Solvents with an olefinic or cyclo-olefinic type of unsaturation: negative test (see 6.5). TABLE 1 - Composition Type Ingredients Percent by Weight I (Clear)
7、Para-phenyl phenol-formaldehyde res in, TT-R-271 25.0 + 1.0 Oil (see 1.2.1 and 3.2) 25.0 1.0 Xylene (TT-X-916, Grade B) 50.0 2.0 II (Clear) Varnish conforming to Type I 50 .o To1 uene (TT-T-548) 50 .O 111 Varnish conforming to Type I 84.0 - t. 0.5 (P i gmen ted) Al uminum Powder (TT-P-320, Type I, C
8、lass B) 16.0 + 0.5 42.0 + 2.0 Class B) 16.0 + 1.0 Varnish conforming to Type I - To 1 uene (TT-T-548) - (Pi gmented) Al um num Powder (TT-P-320, Type I 0 IV 42.0 2.0 3 Licensed by Information Handling ServicesMI L-V-l3750B.(MR) A 3.3 Quantitative requirements. The varnishes shall conform to the quan
9、ti- tative reauirements SDecified in Table II when tested as sriecified in 4.4. Characteristics Type I Type I I Type I I I Type IV Total solids, percent by weight of Pigment, percent by weight of product, Pigments other than aluminum Rosin and rosin derivatives Phenols other than para-phenyl phenol
10、Isooctane insoluble, percent by volume, minimum Drying oils: Grade A Grade B Viscosity, No. 4 Ford Cup, seconds Drying time: product, minimum min mum Air drying, minutes, maximum Set to touch Dry th rough Di rect ional reflectance, percent 48.0 24.0 56.0 35.0 - None Noni? None 50 Tung Li nseed 35-65
11、 30 90 - - None None None 25 Tung Li nseed 10-25 10 60 - 15.5 None None None 50 Tung Linseed 85-200 30 90 15-30 15.5 None None None 20 Tung Linseed 10-25 10 20 15-30 3.4 Oua 1 i tat i ve reau i remen ts . 3.4.1 Condition in container. The clear varnishes from freshly opened full containers chal 1 be
12、 transparent 1 iquids free from moisture, skins or lumps. freshly opened full containers, shall be free from skins or lumps and shall readily mix to a smooth homogeneous state. livering, curdling or gassing in either the clear or aluminum pigmented varnishes when tested as in 4.4.9. The aluminum pig
13、mented varnishes chal 1 not show hard settling in There shall be no evidence of 3.4.2 Accelerated storage stab 1 ity (pigmented type only) When Type I I I and Type IV are tested as in 4.4.10 there shall be no pressure build up. The viscosity of Type III shall not increase more than 10 seconds over t
14、he I viscosity of the material as received. The viscosity of Type increase more than 5 seconds over the viscosity of the origina A spray coat of the varnishes shall show no loss of leafing as a spray coat of the materials as received (visual comparison). 3.4.3 Flexibility. When tested as in 4.4.11 a
15、ll grades and types except Grade B, Type I, II and III shall withstand the bend test without evidence of cracking or flaking. Grade B, Types I, II and III may crack but shall not lift or flake. 4 Licensed by Information Handling ServicesM I L-V- 13750B (MR) 3.4.4 Resistance to boiling water. When te
16、sted as in 4.4.12 Types I and II and the isolated vehicles from Types Ili and IV shall show no wrinkling or bdistering and no more than slight duling or softening immediately after removal from boiling water. When inspected half hour after removal the por- tion of the panel which was imnersed shall
17、be.almost indistinguishable with regard to hardness and adhesion from the duplicate unexposed panel. tendency for a slight whitening to remain shall be disregarded. The 4. QUALITY ASSURANCE PROVISIONS 4.1 Responsibility for inspection. Unless otherwise specified in the con- tract or purchase order,
18、the supplier is responsible for the performance of all inspection requirements as specified herein. Except as otherwise speci- fied in the contract or order, the supplier may use his own or any other facil ities suitable for the performance of the inspection requirements speci- fied herein, unless d
19、isapproved by the Government. The Government reserves the right to perform any of the inspections set forth in the specification where such inspections are deemed necessary to assure that supplies and services conform to the prescribed requirements. 4.2 Sampling, inspection and testing. Unless other
20、wise specified, pling, inspection and testing shall be in accordance with method 1031 Fed. Test Method Std. No. 141. 4.3 Classification of tests. Testing under this specification sha for the purpose of acceptance of individual lots. sam- of 1 be 4.4 Test methods. 4.4.1 Test conditions. The routine a
21、nd referee testing conditions shall be in accordance with section 7 of Fed. Test Method Std. No. 141 except as otherwise specified herein. -. - , . 5 Licensed by Information Handling ServicesMI L-V-l3750B(MR) 4.4.2 The following tests shall be conducted in accordance with appl cable methods of Fed.
22、Test Method Std. No. 141 or as hereinafter specif The right is reserved to make any additional tests deemed necessary to determine that the varnish meets the requirements of this specification - ed TABLE I I I - Index Test Method Applicable Paragraph of Paragraph of method in Fed. this specifica- th
23、is specifica- Test Method tion giving fur- tion giving Tes t s Std. No. 141 ther references requirements Aromatic hydrocarbons Olefinic and cyclo-olefinic compounds Ketones Total solids Pigment Pigments other than aluminum Vehicle isolation Ros i n Phenol i c res ins Isooctane insoluble - Identifica
24、tion of drying oils 7501 viscos i ty 4282 Dry i ng t i me 406 1 5141 Di rect ional reflectance 61 21 Condition in container 301 1 Resistance to boiling water 601 1 Accelerated storage stabi 1 i ty Flexi b i 1 i ty . 622 1 - 4.4.3.2 4.4.3.3 4.4.3.4 4.4.4 4.4.5 - - - - 4.4.6 4.4.7 4.4.8 4.4.9 4.4.10 4
25、.4.11 4.4.12 - - 3.2.1 3.2.1 3.2.1 Table II Table II Table II Table Il - Table I Table I Table I Table I Table I Table t 3.4.1 3.4.2 3.4.3 3.4.4 4.4.3 Solvent analysis for composition L. 4.4.3.1 Separation of volatile portion. Pour about 15 grams of the var- nish into a 50 ml. distilling flask. Add
26、10 ml. of tricresyl phosphate and several anti-bumping stones or Berl saddles. Fit a release valve into the mouth of the flask and attach a delivery tube to the side arm, extending into a receiver consisting of a test tube (20 x 150 mm) with side arm for attaching to a vacuum pump. The glass deliver
27、y tube should reach 1-1/2 inches from the bottom of the tube. Immerse the receiver in a dry ice-acetone bath. Preheat a silicone oil bath to 180C. Raise the oil bath until the oil reaches the sample level. Reduce the pressure slowly to 10 mm. of mercury. After all solvent-has distilled, carefully re
28、lease the vacuum using the valve that is connected to the distilling flask. aromatic solvent determination and the test for ketone, olefinic and cyclo- o1 ef i n i c compounds. Reserve the collected distillate for the 6 Licensed by Information Handling ServicesMIL-V-23750B 80 m 9999906 0498069 7 m M
29、I L-V-l375OB(MR) 4.4.3.2 Determination of aromatic hydrocarbons. Apparatus: A gas chromatograph equipped with a thermal conductivity detector. Column Preparation: Two lengths of 1/4-inch copper tubing, 6-ft. and 18-ft. long, are packed with 35% N,N-Bis(2-cyanoethyl) formamide on 60- to 80- mesh Chro
30、mosorb P. Operating Conditions: 6-ft. 18-ft. Detector cell temperature, OC. 300 Detector cell current, ma. 150 inject ion port temperature, C. 300 Helium flow at exit, cc/minute 175 Column temperature, OC. 125 300 150 300 110 1 O0 4.4.3.2 of distil add exact graduate 1 Total aromatic content - proce
31、dure A. Transfer prec ate or thinner to a 25-ml. glacs-stoppered volumetric f y 0.3 ml. of high purity phenylcyclohexane. While cool nder tap water, add 15 ml. of 85% sulfuric acid slowly. sely 3 ml. ask and ng the After all the acid has beenadded,?shake vigorously for 2 minutes and allow the layers
32、 to separate. Add sufficient 85% acid to force the top layer into the neck of the flask and then transfer most of the top layer to a micro-separatory funnel. all acid has been removed and reserve the washed solvent for chromatographic analysis. Install the 6-ft. column and follow the operating condi
33、tions described above. Inject about 5 microliters of the acid-treated sample and al low the chromatogram to develop unti 1 the internal standard, phenylcyclo- hexane , eme rges . Wash the distillate with 5 ml. portions of distilled water until % total aromatic solvents, v/v = A X lof; X l.O7f:f; B w
34、here, A = area of aromatic solvent peaks B = area of internal standard peak * = percent of internal standard f:;! = detector response correct ion factor NOTE: If the above determination exceeds 8 percent, continue with the fol lowing procedure: Licensed by Information Handling ServicesMIL-V-l3750B(M
35、R) 4.4.3.2.2 Toluene and ethylbenzene - procedure B. Treat 3 ml. of sol- vent in the same manner as described in procedure A except substitute benzene for phenylcyclohexane. Install the 18-ft. column and follow the operating conditions described for that column. Inject about 3 microliters of sample
36、and allow the chromatograph to develop until all of the xylene isomers appear. 12OoC. ture to 100C. Purge the column by raising the column temperature to After the high boiling materials emerge, reset the column tempera- Calculate the percent of toluene and ethylbenzene as % toluene, v/v = (area of
37、toluene peak)(l.017)9: (lo)* (a rea of benzene peak) % ethylbenzene, v/v = (area of ethylbenzene peak) (1.054);: (lo)* (area of benzene peak) where, is the correction factor for the detector response *;: is the percentage of internal standard added Sensitivity of the instrument should be adjusted to
38、 keep peaks from running off the scale. changes in sensitivity when computing the peak areas. NOTE: Appropriate corrections must be made for 4.4.3.3 Test for olefinic or cyclo-olefinic compounds. and place 2 drops of the distillate in each. Dissolve the first sample in 1 ml. of carbon tetrachloride
39、and add 1 drop of 1 percent bromine in carbon tetrachloride. Shake and allow to set for 5 minutes. A positive test is indicated by the complete absence of yellow color when observed against a white background. Dissolve the second sample in 1 ml. of acetone and add 1 drop of 1 percent permanganate so
40、lution (1 gram of potassium permanganate crystals in 95 mls. of acetone and 5 mis. of water). for 2 minutes. A positive test is indicated by the decolorization of the purple solution. The solvent is considered to fail the test for olefinic and cyclo-olefinic compounds if either of the above tests is
41、 positive (see 3.2.1 and 6.5). Take 2 test tubes Shake and al low to set 4.4.3.4 Test for ketones. 4.4.3.4.1 Reagent. Two grams of 2,h-dini trophenylhydrazine -I- 4 mlc. of concentrated sulfuric acid + 30 mls. methanol (add slowly) + 10 mls. water. 4.4.3.4.2 Procedure, Pipette 1 ml. of reagent into
42、a 20 x 170 mm. test tube. A yellow precipitate or cloud in the reagent layer indicates the presence of ketones. Add 10 drops of distillate (see 4.4.3.1) and shake for 30 seconds. Run a blank using one ml. of reagent and 10 drops of mineral Licensed by Information Handling ServicesMIL-V-13750B 0 m 99
43、97906 0478071 7 m - MI L-V- 137508 (MR) 4.4.4 Pigment determination. Using a 10 cc. syringe transfer an 8 to 10 gram sample of the thoroughly mixed varnish to a 250-ml. beaker. Determine the weight of the sample to the 0.001 gram by differenceusing the weight of the syringe and varnish and the weigh
44、t of the syringe after discharging the varnish. Add 150-ml. of the benzol to the beaker and stir thoroughly-. Fil- ter the mixture through a tared 30-ml. fritted glass filtering crucible hav- ing a medium porosity. a stream of benzol. Thoroughly wash the residue in the crucible first with benzol and
45、 then with acetone. Dry at 100“ to 105C. for one hour, cool in a desiccator and weigh. Calculate the percent piqment in the sample from the Wash any residue in the beaker into the crucible with increase in weight-of the crucible. subsequent sodium hydroxide solubi 1 ity test. Save theekracted alumin
46、um pigment 4.4.5 Pigments other than aluminum. Weigh an approximate 0.5 gm. samp of the isolated pigment (from 4.4.4) and transfer to a 600-mi. Erlenmeyer flask. Add 300-1111. of 0.1 normal sodium hydroxide solution. Stopper and shake the flask frequently during a one half hour period. Release the s
47、t per while the material is at rest to permit escape of hydrogen gas. Note whether any insoluble material is present. A slight cloud which does not or e P- settle out on standing may be observed. Gooch crucible. From the increase in the weight of the crucible and the weight of the origi- nal sample
48、calculate the percent insoluble in 0.1 Normal NaOH as follows: Filter imnediately through a tared Wash thoroughly with hot water and dry to constant weight. Wt. of 0.1 Normal NaOH insoluble X 100 Weight of sample Any amount of 0.1 Norma.1 NaOH insoluble in excess of 2.0% shall be consid- ered pigmen
49、t other than aluminum. 4.4.6 Isooctane insoluble. Into a 500 ml. graduated centrifuge tube pour exactly 10 ml. of isooctane. Add exactly 10 ml. of the clear varnish or iso- lated vehicle. Fi 11 the tube with isooctane, stopper and agi tate thoroughly, centrifuge in ml. Multiply ml. by ten and report as percent isooctane insoluble. for approximately one hour and read the insoluble (bottom layer) 4.4.7 Identification of drying oils. Extract the fatty acids as in methods 7021 and 7031 of Fed. Test Method Std. No. 141 and identify the drying oi
