1、RIL-E-24617A 9999906 2003752 780 IHETRICJ MIL-E-24617A(SH) 1 June 1995 SUPERSEDING 10 March 1983 (See 6.7) MIL-B-24617 (SH) MILITARY SPECIFICATION EDTA HARDNESS TESTING REAGENTS, BOILER FEEDWATER, SHIPBOARD USE This specification is approved for use by the Naval Sea Systems Command, Department of th
2、e Navy, and is available for use by all Departments and Agencies of the Department of Defense. 1. SCOPE 1.1 ScoDe. This specification covers the composition and quality of reagent chemicals used for testing hardness in shipboard boiler feedwater. 2. APPLICABLE DOCUMENTS 2.1 Government documents. 2.1
3、.1 SDecifications. standards. and handbooks. The following specifi- cations, standards, and handbooks form a part of this document to the extent specified herein. those listed in the issue of the Department of Defense Index of Specifications and Standards (DODISS) and supplement thereto, cited in th
4、e solicitation (see 6.2). Unless otherwise specified, the issues of these documents are SPECIFICATIONS FEDERAL A-A-20135 - Sugar, Refined and Sugar, Brown. PPP-C-2020 - Chemicals, Liquid, Dry, and Paste: Packaging of. I Beneficial comments (recommendations, additions, deletions) and any pertinent da
5、ta which may be of use in improving this document should be addressed to: Commander, SEA 03R42, Naval Sea Systems Command, 2531 Jefferson Davis Hwy, Arlington, VA 22242-5160 by using the self-addressed Standardization Document Improvement Proposal (DD Form 1426) appearing at the end of this document
6、 or by letter. AMSC N/A FSC 6810 DISTRIBUTION STATEMENT A. Approved for public release; distribution is unlimited. Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-MIL-E-24bL7A 9999706 2003753 bL7 MIL-E-24617A(SH) STANDARDS FEDERAL FED-STD-313 - Mater
7、ial Safety Data, Transportation Data and Disposal Data for Hazardous Materials Furnished to Government Activities. MILITARY MIL-STD-129 - Marking for Shipment and Storage. (Unless otherwise indicated, copies of federal and military specifications, standards, and handbooks are available from the Stan
8、dardization Documents Order Desk, BLDG. 4D, 700 Robbins Avenue, Philadelphia, PA 19111-5094.) 2.1.2 Other Government documents. drawings. and Publications. The following other Government documents, drawings, and publications form a part of this document to the extent specified herein. Unless otherwi
9、se specified, the issues are those cited in the solicitation. DEPARTMENT OF LABOR (OSHA) Code of Federal Regulations (CFR) CFR 29, Part 1910.1200 - Hazard Communication Standard. DEPARTMENT OF TRANSPORTATION (DOT) Code of Federal Regulations (CFR) CFR 49, Part 100-199 - Hazardous Material Regulation
10、s. (Application for copies should be addressed to the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402.) 2.2 Non-Government Publications. The following document(s) form a part of this document to the extent specified herein. Unless otherwise specified, the issues of
11、 the documents which are DOD adopted are those listed in the issue of the DODISS cited in the solicitation. Unless otherwise specified, the issues of documents not listed in the DODISS are the issues of the documents cited in the solicitation (see 6.2). AMERICAN CHEMICAL SOCIETY (ACS) Specifications
12、 - Reagent Chemicals. (Application for copies should be addressed to Applied Publications, American Chemical Society, 1155 16th Street, NW, Washington, DC 20036.) AMERICAN SOCIETY FOR TESTING AND MATERIALS (ASTM) D 1126 - Standard Test Method for Hardness in Water. (DoD adopted) D 1193 - Standard Sp
13、ecification for Reagent Water. (DoD adopted) D 3082 - Standard Test Method for Boron in Water. D 3113 - Standard Test Methods for Sodium Salts of EDTA in Water. D 4192 - Standard Test Method for Potassium in Water by Atomic E 1252 - Standard Practice for General Techniques for Qualitative Absorption
14、 Spectroscopy. Infrared Analysis. 2 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-(Application for copies should be addressed to the American Society for Testing and Materials, 1916 Race Street, Philadelphia, PA 19103.) AMERICAN PUBLIC HEALTH ASSOC
15、IATION (APHA) Standard Method 4500-S2- Sulfide (Application for copies should be addressed to the American Public Health Association, 1015 Fifteen Street, NW, Washington, DC 20005.) AMERICAN ASSOCIATION OF TEXTILE CHEMISTS AND COLORISTS (AATCC) Colour Index, 3rd Edition, Volume 1-4: The Society of D
16、yers and Colourists, Bradford, England and American Association of Textile Chemists and Colorists. 1971. (Application for copies should be addressed to the American Association of Textile Chemists and Colorists, P.O. Box 12215, Research Triangle Park, NC 27709.) (Non-Government standards and other p
17、ublications are normally available from These documents also the organizations that prepare or distribute the documents. may be available in or through libraries or other informational services.) 2.3 Order of Drecedence. In the event of a conflict between the text of this document and the references
18、 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. 3. REQUIREMENTS 3.1 Reagent material aualitv. Materials used in the manufacture of each of the reagents covered by t
19、his specification shall conform to all applicable specifications of the American Chemical Society (ACS)(If Eriochrome Black T cannot be obtained as ACS Grade, it shall conform with ACS specifications set forth in Reagent Chemicals). Reagent solutions shall be prepared using reagent water which confo
20、rms to ASTM D 1193, type III. shall be provided to the Government laboratory with lot acceptance test samples (see 4.2.3 and 6.3). Manufacturer and lot number for all reagents 3.1.1 Hardness titrating solution. The hardness titrating solution shall be an aqueous solution of 0.01 Molar (M) disodium e
21、thylenediaminetetraacetate, dihydrate (Na2EDTA*2H20). 10.5 f 0.1 by the addition of sodium hydroxide. 4.4.1, the concentration of Na2EDTA*2H20 shall be 3.72 f 0.07 gram per liter (g/L). (mg) of calcium carbonate (Caco,). ) The pH of the titrating solution shall be adjusted to When tested as specifie
22、d in (1.0 milliliter (mL) of 0.01 M Na2EDTA*2H,0 solution equals 1.0 milligram 3.1.2 Hardness buffer. The hardness buffer shall be a dry powdered water soluble uniform mixture formulated as specified in table I. accordance with A-A-20135, type I, class 3. The hardness buffer solution (0.185 k 0.050
23、grams in 100 mL of reagent water) shall range in pH from 9.9 to 10.4. Sucrose shall be in 3 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-E-24bL7A D 999990b 2003755 49T M Characteristic Sodium tetraborate, decahydrate . Percent TABLE I. Hardne
24、ss buffer formulation. I I i Potassium hydroxide (KOH), 86% Sodium sulfide (Na$), anhydrous 4.0 1.0 (Na$,O,* 10HzO) 8.0 I Sodium tetraborate, decahydrate Potassium hydroxide Sodium sulfide, anhydrous 7.5 8.8 2.4 4.0 0.3 1.0 I Sucrose Remainder 1 3.1.2.1 CornPosition. When tested as specified in 4.4.
25、2, the hardness buffer shall conform to table II. spectroscopy (IR). Sucrose shall be qualitatively identified by infrared Characteristic Eriochrome Black T TABLE II. Hardness buffer analvtical reauirements. Percent Minimum . Maximum 0.25 0.50 Percent I Characteristic 3.1.2.2 Performance. When teste
26、d as specified in 4.4.3, the hardness shall be 1.0 f 0.02 equivalents per million (epm). 3.1.3 Hardness indicator. The hardness indicator shall be a dry, water soluble, uniform mixture of Eriochrome Black T (EBT), colour index 14645, and sucrose in accordance with A-A-20135, type I, class 1. The har
27、dness indicator shall conform to table III and at a pH of 9.9 to 10.4 shall impart a red color to a water sample containing hardness and a blue color when hardness is absent. 3.1.3.1 Comosition. When tested as specified in 4.4.4, the EBT hardness indicator shall conform to table III. by IR. Sucrose
28、shall be qualitatively identified TABLE III. Hardness indicator reauirements. Sucrose Remainder I I 4 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,- MIL-E-24bL7A = 9999906 2003756 326 = MIL-E-24617A(SH) 3.2 Material safetv data sheet. The contracti
29、ng activity shall be provided a material safety data sheet (MSDS) at the time of contract award. The MSDS shall be provided in accordance with the requirements of FED-STD-313. The MSDS shall be included with each shipment of the material covered by this specification (see 5.4 and 6.4, including lot
30、acceptance test samples, see 4.2.3). 4. QUALITY ASSURANCE PROVISIONS 4.1 ResDonsibilitv for insDection. Unless otherwise specified in the contract or purchase order, the contractor is responsible for the performance of all inspection requirements (examinations and tests) as specified herein. Except
31、as otherwise specified in the contract or purchase order, the contractor may use his own or any other facilities suitable for the performance of the inspection requirements specified herein, unless disapproved by the Government, The Government reserves the right to perform any of the inspections set
32、 forth in this specification where such inspections are deemed necessary to ensure supplies and services conform to prescribed requirements. 4.1.1 ResDonsibiitv for comDliance. All items shall meet all requirements of sections 3 and 5. The inspection set forth in this specification shall become a pa
33、rt of the contractors overall inspection system or quality program. The absence of any inspection requirements in the specification shall not relieve the contractor of the responsibility of ensuring that all products or supplies submitted to the Government for acceptance comply with all requirements
34、 of the contract. Sampling inspection, as part of the manufacturing operations, is an acceptable practice to ascertain conformance to requirements, however, this does not authorize submission of known defective material, either indicated or actual, nor does it commit the Government to accept defecti
35、ve material. 4.2 Oualitv conformance inspection. Quality conformance inspection shall consist of the lot acceptance testing of 4.2.2 and the inspection of 4.5 (see 6.3). 4.2.1 Lot_. For purposes of examination, testing and inspection, a lot shall consist of all reagents manufactured in a single prod
36、uction run and submitted for inspection at one time. 4.2.2 SamDlinP for lot acceptance testing. From each lot, three sample filled containers shall be randomly selected and subjected to the examination of 4.3 and the tests of 4.4 (see 6.6). One gram of Eriochrome Black T shall be submitted with the
37、inspection samples of hardness indicator. 4.2.3 Test laboratory. When specified (see 6.2), the samples selected in 4.2.2 shall be forwarded to a laboratory satisfactory to NAVSEA (see 6.5). 4.3 Examination of filled containers. Each sample filled container selected as specified in 4.2.2 shall be ins
38、pected to verify compliance with all require- ments of this specification regarding fill, closure, marking, and other require- ments not involving tests. Containers shall be examined for defects of the container and closure, for evidence of leakage, for unsatisfactory markings, and for the required
39、amount of reagent. 5 Provided by IHSNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-4.4 Tests. Unless otherwise specified in the test procedure or method, references to reagent water shall mean ASTM D 1193, type III. testing shall conform to all applicable ACS spec
40、ifications. Reagents used in 4.4.1 Hardness titrating solution. Use pipet and transfer a 100 mL aliquot of the hardness titrating solution to be tested to a l-L volumetric flask. Dilute to the mark with reagent water and mix thoroughly. dilute hardness titrating solution in accordance with ASTM D 31
41、13, test method B, using standard solution magnesium A. Calculate the concentration of NaZEDTA*2H20 as follows with TA and S as defined in section 22.1 of method ASTM D 3113: Test a 100 mL volume of the TA x 1000 Na2EDTA*2H,O (g/L) = 4.4.2 Hardness buffer comDosition. A 0.200 i: 0.001 gram sample of
42、 the hardness buffer shall be dissolved in 1 L of reagent water and analyzed for potassium and boron by inductively coupled plasma (ICP) or direct current plasma (DCP) atomic emission spectroscopy (AES). Alternate test methods are ASTM D 4192 for potassium and ASTM D 3082 for boron when using a 1:l
43、dilution of the 200 milligram per liter (mg/L) buffer solution. The sulfide ion shall be analyzed in accordance with APHA Method 4500-S2- on the 200 mg/L solution of the hardness buffer. Calculate the composition of the buffer as follows: Percent KoH = Potassium, mg/L x 1.43 x 100 200 Sulfide, mg/L
44、x 2.44 x 100 200 Percent Na$ = The sucrose shall be identified qualitatively by IR. hardness buffer and potassium bromide (Ur) shall be used to prepare a KBr pellet for an IR spectrum in accordance with ASTM E 1252. A finely ground mixture of 4.4.3 Hardness buffer Derformance. Hardness buffer perfor
45、mance shall be determined in accordance with ASTM D 1126 by measuring the hardness of a 100 mL sample prepared by dissolving 0.055 f 0.005 grams of dried calcium chloride (CaClt) in 1 L of reagent water. ASTM D 1126, add 0.185 f 0.050 grams of the hardness buffer to be tested to the CaC1, sample sol
46、ution prepared for use in section 9. hardness, determine the hardness as in section 10.1. (A standard class A buret may be used instead of the microburet.) In place of the buffer of section 7.4 of method Using the procedure for low 6 Provided by IHSNot for ResaleNo reproduction or networking permitt
47、ed without license from IHS-,-,-HIL-E-2YbL7A b 2003758 LT = MIL-E-24617A(SH) 4.4.4 Hardness indicator. Weigh 2.000 grams of the hardness indicator to be tested to the nearest 0.001 gram. Record the weight. 1-L volumetric flask and dilute to the mark with reagent water and mix thoroughly. Weigh 0.100
48、 i 0.001 grams of Erichrome Black T (EBT). Transfer the EBT to a 1-L volumetric flask and dilute to the mark with reagentwa- ter and mix thoroughly. Pipet and transfer 4 mL, 6 mL, 8 mL, 10 mL and 12 mL, respectively, of the EBT stock solution to 100-mL volumetric flasks. the mark with reagent water
49、and mix thoroughly, (W/VIS) spectrophotometer and 10 mm matched silica cells, measure the absorbances of the above standard solutions at a wavelength of 503 nanometers. concentration of the EBT in the hardness indicator directly from the calibration curve by linear regression. Calculate the percent EBT as follows: Transfer the sample to a Record the weight. Dilute to Using an ultraviolet/visible Determine the EBT, ppm x 100 Weight of sample x 1000 P
