1、 . I . ,.-.-.-.- - u . “ . . . . .- . I .-._. . - , . - ,.- . b . . I. . , ?. . . . -.-.- . ,. . _ I:-:.:.:.:.:. , .-. . ,._-. -. . . . . . . . . . . . . -.- . .- -.- . I .- . . “ . . . . . -. . . . - . . . . . . , . . . .-. . - . -.-.-. - cl_-.* -. _.-. . . -*.-.+ LTZ.:z:-:, b-.-*.- . I._ ._ .- r-
2、-.-.- I_ . Ce _. ,_._I._ .-.- I _ . - - 4. -. . .- - “ “ . . _.- I _-.- . . - .- . . -., “._-. - . - -.- - . _ . I . . i L/ :.-:.x.x: .-. . ,. . _.- . . .- . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-VIL-L-BOb7A 80 W 9999906 0098872 2 c M1t-806
3、7.4( USAF) (Copies of specifications, standards, drawings, and publications required by contractors in connection with specific procement functions should be obtained from the procnring activities or as directed by the contracting officer . ) 3. IIEQlITRDENTC 3.1 The leather dressing furnished under
4、 this specification shall be a product which has been tested and has passed the qualification tests sFecified here in . 3.1.1 Approval for Treated Leather The approval of the Surgeon General, BAF, shall be obtained by procuring activity before procurement of leather materials containing mildew-resis
5、tant treatment for uses which will involve intimate prolonged contact with the skin of mAF personnel, 3,2 Materials.- The materials used in the manufacture of the leather dressing shall consist of a mixture of oil (vegetable, animl, mineral, synthetic), fungicide and solvents in such proportions and
6、 of such physical characteristics as to meet the requirements of this specification. 3.21 “he manufactured leather dressing shall be a stable, honogeneous sslutiori. 3.2.2 Leather dressing, mildew-preventive, shall be purchased by volume, the unit being a U. S. gallon at 25OC. 3.3 Type I - Orthophen
7、ylphenol Fungicide 3.3.1 Composition,- The percentage by weight for type I leather dressing shall conform to the requirements in table I. TABiE I Percentage by %eight of Ingredients Leather Dressing %e 1 Ckthophenylphenol 4.8 Gmpow,ded Vegetable Oil 9.6 Hydrocarbon Solvmt 85.0 5.3 10.4 88 .o 3.3.2 I
8、ngredients.- Ingredients used in the manufacttzre of type I leather dressing shall conform t3 the requirements specified below when tested by _applicable methods described in 6.3. 2 . . . . . . . . I . . k:. ci: . . i . , . r-.z . . -.- . . I. . _ . -. _- . . i b _. ,.- . I ,. . . ,.-.- . -. , . , .
9、 . : -. ,- . , . . Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-EIIL-eition Ehaber Flash Foint Ibrciiry Copper Sediment 1-31dew growth Chlorine 8lfw 0.850 -.i- 13% 16% Neutral Acid 0.3 105OF None None Trace Slight 0.654% 0.7500% 0.654% 0 7500% 3.3
10、.3J Pieces of vegetable tanned leather shall be treated with type I Leather dressing and shall contain a maximum of 1.6 percent by weight of orthophenylphenol for uso in the mildew growth teat in table IV, A alight amount of mildew growth shall consist of the appearance of fungi along the cut edges
11、of the specimens and not more than 2 percent of the exposed surface. The leather selected for treatment with type I leather dressing and for use as imtreated leather shall contain no fungicide. 3.3.3.1.3. The percefit orthophenylphenol in the treated leather shall be determined by scs.ecting 2 rando
12、m samples of treated leather and 2 samples of untreated leather. Each original sample shall weigh approximately 5 grams. Keeping samples separate, cut each sample into small pieces approximately 1 mm sqwe or grind in a Wiley Mill and dry for 16 hours at 4OOC. These samples shall be tested for percen
13、t orthophenylphenol in accordance with 11.3.1.1, ,- A lot shall consist of the leather dressing manufactured under essentially the same conditions and submitted for inspection at substan- tisslly the same time, be selected at random from each lot, shall be mixed to constitute 1 gallon of the leather
14、 dressing, for testing shall be subjected to the tests listed below an6 described under 4.3 test methods, ,2,1,2 Sampling Plan,. The following number of sample containers shall. Equal portions of each sample container The 1 gallon No. of con tainers in lot, No. of sample c ontaine rs 9 or more 8 or
15、less 8 all a. Type I, orthopbpnylphenol fungicide, leather dressing (1) Orthophenylphenol determination (2) Specific gravity Type II, optional fungicide, leather dressing (2) Unsaponif iable matter Type I and Type II leather dressing b, (1) Oil c. Nonvolatile residue Neutralisation number mash point
16、 Mercury Copper Sediment Resistance to mildew growth Chlorine Sulfur 4,2,L2.2 Rejection and Retest,- When the 1 gallon sample container fails the specified tests, this is cause for rejection of the lot, Before resubmitting the lot, the contractor shall fully explain to the inspector both the correct
17、ions made and cause of previous rejection. 4.2.2 Defects in Items Already Accepted.- The investigation of a test fail.ure could indicate that defects may exist in items already accepted, the contractor shall fully advise the procuring activity of ail defects likely to be found, and methods of correc
18、ting them, If so, 6 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-BOb7A 80 = 7777706 0078877 L 4.3 Test Methods 4.3.1 Type I, Orthophenylphenol Fungicide, Leather Dressing 4.3.1.1 Orthophenylphenol Method I.- This method may be used for deter
19、mination of percent of orthophenylphenol in the treated leather and for percent purity of the orthophenylphenol to be used in the leather dressing only. 4.3.1.1.1 The materials for method I shall be as follows: a. Anhydrous Diethyl Ether, CP. be The indicator solution for method I shall be as follow
20、s: 450 milligrams of anhyrous CP titanium dioxide shall be dissolved in 1 liter of concentrated sulfuric acid, specific gravity le84. (This requires heating for 8 hours). The resulting solution shall be clear and have a small but constant optical density through the 350-800 millimicron region. C. Gr
21、thophenylphenol, 100 milligrams in 100 milliliters of diethyl ether . 4.3.i.i.2 The equipment for method I shali. consist of: 1 1 - Colorimeter - The Cary Model11 spectrophetometer, The Beckman - 25 ml burette and stand DU spectrophotometer or equal type are satisfactory 4 - i25 ml flasks 4 - 250 ml
22、 beakers 1 - 100 ml volumetric flask 4 - normal funnels and stands 4.3.i.3 The procedure for method I shall be as follows: a. From each ground, treated-leather sample take a random portion of such weight that the calculated amount of orthophenylphenol shall be between 1 and 3 milligrams in each samp
23、le to be analyzed. the leather contains from 1.0 to 3.5 percent orthopheaylphenol a 0,100 gram sample shall be recommended.) (For example if b. Each sample shall be placed in a separate, properly labeled, 125 ml flask. To each flask add 25 ml of anhydrous ether. The flasks shall be stoppered and all
24、owed to stand overnight or about 16 hours. The ether extract shall be decanted through suitable filter paper into 250 ml beakers. A second extraction shall be made by adding i5 ml ether to each sample and shaking occasionally for 15 minutes an decanting the liquid to the first extraction. fungicide
25、is removed fiom the leather. A third and similar extraction shall -insure that all of the Evaporate the ether with or without the 7 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-L-BOb7A BO a 94949Ob 0098878 3 MIL- Ti8C67A ( USAF) aid of vacuum
26、but no heat shall be used, vacuum is used until about 10 ml of concentrated extract remains, These last few milliliters shall be evaporated under room conditions, about 2OoC, without the uso of vaccuum to avoid- loss of the orthophenylphanol that remains in the res5due , !Id 25 ml of the titanium sy
27、rup at 2OoC to the fungicide residue and stir the resulting solution for 5 minutes, added immedr;ately after the ether is evaporated and water shall be absent since it reduces the optical density of the reslxlting titanium-phenol cornple%. After abou.1; 15 minutes the titani-m-phenol mjxture shall b
28、e placed in a suithble cell and examineci with the spectrophotometer at 455 miliimicrons. complex is stable up to 2 hours,) The average optical density of the extract from the untreated leather shall be subtracted from the average optical density of the extract from the treated leather an this shall
29、 be used to determine the concentration of orthophenylphenol in the leather from a standard curve, prepared, taken for the desired amounts of phenol. and 25 ml of the titanim syrup ad.ded to the residue as described a3ovo. on standard cross section paper as a function of the concentration of orthoph
30、enylphenol. The evaporation shall contiaue if c, The titanium syrap shall be (The titanium-phenol d. e. A standard curve for O-,$nilligrams orthophenylphenol shall be Using stock solution described in 4.3,l,l,lc, aiiquots shall be The ether solvent shall be evaporated f. The optical density values a
31、t 4.55 millimicrons shall be plotted #je Frequeet checking of the standardization curve is recomnended. 4,3.1,2 Orthophenylphenol Ylthod 11,- This method may be used for deter- rnlnation of percent of orthophenylphenol in the leather dressing, for percent in the treated leather, and for percent puri
32、ty of the orthophenylphenol to be used in the leather dressing, from nonvolatile substances by steam distillation for accurate determination of the orthophenylphenol content. This method requires the separation of orthophenylphenol 4*3,1,2,1 Steam distillation for Ikthod II 4,3,1.2.l,J Materials for
33、 steam distillation shall be as follows: a, Orthophosphopic acid solution - Approximtel 25 percent (85 percent acid, reagent grade, diluted 1:4 5 Sodium hydroxide solution - Two grams of reagent grade sodim h3droxide in 100 ml of distilled water. b. 8 Provided by IHSNot for ResaleNo reproduction or
34、networking permitted without license from IHS-,-,- MIL-L-Ob7A AO 7977706 0078877 5 M MILUO67a( U5A.F) +.?.l.2al.2 Ekuipent for stem distillation shall be as follows: 1- Steam distillation setup fitted with glass joints. It should consist of a 1 liter steam flask connected to a 1 liter sample flask,
35、which is in turn connected to a condenser with a standard 10 inch coil wlth fwmcl and stopcock at top 1- 500 ml volumetric flask 1- aririg blender or equal type 4.3.1.2.1.3 a. The procedure for steam distillation shall be as follows: Place 1 gram of the leather dressing or the mound sample which- ev
36、er is applicable into a Waring blender. 50 to IGO ml of distilled water. After the sample is well slurried, transfer to the sm,ple flask, add 10 ml of dilute orthophosphoric acid and a mirijmum amourit of water (about 100 to 30 mi) to insure effective steam distillation. Add 5 ml of 1 N sodium hydro
37、xide and b, To the condenser funnel add 10 ml of 2 percent sodium hydroxide solutton. t2. fits well into the neck of the flask. hydroxit. to run 6own the cordlenssr tubing into the flask so as to wet the sides of the flask well. Place a 500 ml volumetric flask under the cordanser tip so that the All
38、ow 1 to 2 ml of the dilute sodium C. Add 800 to ?O ml of distill-e water to the steam flask and Heat the steam flask until the sample flask connect to the sample flask. begins to boil, then tho sample flask may also be, heated to keep the liqutd volme low. The condensate should come through fairly c
39、ool in any case. d. Collect 500 ml of distillate. If oil or wax 6istills over, it is disregarded in taking the aliquot. keep th orthophenylphenol in the aqueous phase. The solution should be alkaline enough to 4.3.1.2.2 Orthophenylphensl Deternlnation for bthd II 4.3.1.2.2.1 The materials for method
40、 II shall be as follows: a, Indicator Sslution for method 11 - Dissolve 0.030 gram of 2.oquktionechlorsimider ir1 25 ml of 95 percent ethyl alcohol. Mako to volume with 95 percent ethyl alcohol in a 50 ml low actinic glass volumetrie flask . b, Buffer Salution.- Dissolve 15 grams of anhydrous sodium
41、 tetraborate powchr in 900 ml of warm distilled water. to prevent lunping. solution (20 to 40 percent), to volwm. water should have a pH of 9.6. buffer shoulcl be adjusted. Stir vigorously wh5le adding powder Add 3.27 grms of sadiuni hydroxide in the form of a strong Transfer to a 1000 ml volumetric
42、 flask and make If tho pH differs by more than 1.10, then the Five ml of the buffer solution when diluted to 100 ml with distilled 9 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-c. Copper sulfate solution.- Dissolve 0,050 gram o, copper sulfate (C
43、u SO 5 HzO) in 50 ml of water. an EI td e to volume. Transfer to a 1800 ml volmetric flask C. Orthophenylphenol stmdard solutions for method II.= Dissolve 1 gran of orthophenylphnol in 1C to 15 iii3. of 1 N sodim hydroxide, transfer to a 10CQ ml volmetric flask and bring to volme with distilled wate
44、r (solution A). This solution 1s good for only a week. daily. Dilute 1CO ml of solution A to 1 liter, 100 micrograms per: ml (solution 3). 1 microgram of orthophenylphenol (solution C) . The following solu.tj.ons must be prepared Then dilute 1C ml of solQtion B to 1 Liter, 1 ml contains 4.3,1,2.2.2
45、“he equipment for method II shaU be as follows: a. Photonetrfc determination,- One photometric instrument for color measurement, with ten absorption cells (curvettes) of 40 mm light path and ten 30 nil wo1metrj.c flasks. b, Visual. determination.- Ten 1CO ml matched Nessler tubes with white Sased co
46、raparison rack. C. 1 - 50 ml low actinic glass volumetric flask 5 - 1000 mL volumetric flasks 1 - 25 ml graduated pipette 1 - 25 ml burette and stand 4,3c1.2.2.3 The procedure for method II shall be as follows: a. From the steam distillate of each sqle as specified in 4.3.1.2.1 pipette into separate
47、 100 ml volmetric flasks an aliquot of such volwne so that the calculated amount of orthophenylphenol shall be at least 5 milligrams or more. solv.tion, Shake and dilute to about 90 ml. with distilled water. burette add 1 ml of tho indicator solution for method II, shake, and make to volwi:, and mix
48、 again. b. 1 hour, difference in room temperature, 25, 50, and 75 ml of orthophenylphenol standard solution C and 1 ml of solution II and follow the same procedure as described in a. above. Ad 5 mi of buffer solution and 1 ml of the copper sufate bom a Allow solutions to shnd in a dark plaoe at room
49、 temperature for It is advisable to prepare several standard curves, one for each 5OC To prepare the standard curve use O, 5, 10, C. Photorretric determination.- Using a suitable colorheter, aero the instrument on the reagent blank, and measure the percent transmittancy and conpare to the standard curve platted on semilog paper fer that temperature, Using a 4
