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1、ANSI PW4.185-1987 A N S I P“4*185 87 072435U 003a1265 3 F-35-19 Revision of ANSI PH4.185-1980 for photography (chemicals) - Page 1 of 5 pages I Warning and Safety Precautions Some of the chemicals specified in the test proce- dures in this standard are corrosive, toxic, or otherwise hazardous. Speci
2、fic caution, warning, and danger notices are given in the footnotes but, in addition, the normal precautions required dur- ing the performance of any chemical procedure must be exercised at all times. It is recommended that anyone using these chemicals obtain from the manufacturers pertinent informa
3、tion about the hazards, handling, and use of these chemicals. Such information is usually furnished by the chemical manufacturer in the form of a material safety data sheet (OSHA Form 20 or equivalent). I Introduction (This Introduction is not part of American National Standard PH4.185-1987 ,) This
4、standard is one of a series that establishes the min- imum criteria of purity for chemicals used in processing photographic materials. Although the ultimate criterion for suitability of photographic-grade chemical is its successful perfor- mance in an appropriate use test, the shorter, more economic
5、al tests described in this standard are gener- ally adequate. This standard is a revision of American National Standard Specification for Photographic Grade Ethylenediaminetetraacetic Acid (EDTA) (Ethylene- dinitri1o)tetraacetic Acid , and Its Salts, ANSI PH4.185-1980. In this latest revision, the s
6、ection on “Reagents for Test Methods” has been renamed “Reagents, Materials, and Glassware.” The strength of standard solutions is now expressed as molarity. Also, minor changes in precaution notations have been made, and the general format has been changed to be in agree- ment with the style outlin
7、ed in the Directives for the Technical Work of the International Organization for Standardization (ISO). 1. Scope This standard establishes the criteria for the purity of photographic-grade ethylenediaminetetraacetic acid (EDTA) and its salts, and describes the tests to be used ationai Standard may
8、be revised or withdrawn at any time. The procedures of the American National be taken to reaffirm, revise, or withdraw this standard no later than five years from the date of ap- ai Standards may receive current information on au standards by calling or writing the American Na- , American National S
9、tandards Institute, 1430 Broadway, New York, N.Y. 10098 ANSI SC48714 - Copyright American National Standards Institute Provided by IHS under license with ANSI Licensee=USN Ship Repair Facility Yokosuka/9961031100 Not for Resale, 05/09/2007 01:34:14 MDTNo reproduction or networking permitted without
10、license from IHS -,-,- ANSI PH4.385 87 m 0724350 00112bb 5 H Page 2 of 5 pages to determine the purity. The salts included are diso- dium ethylenediaminetetraacetate dihydrate, tetra- sodium ethylenediaminetetraacetate dihydrate, tetra- sodium ethylenediaminetetraacetate solution, tetra- potassium e
11、thylenediaminetetraacetate solution, and diammonium ethylenediaminetetraacetate solution, hereafter respectively referred to as: Naz EDTA*2Hz O Na4 EDTA*2Hz O Na4EDTA solution K4 EDTA solution (NH4)2EDTA solution 2. General Information 2.1 Physical. EDTA, NazEDTA*2H20, and Na4EDTA *2Hz O exist in th
12、e form of white crystalline powders. The three solutions exist as off-white aqueous solutions. The chemical formula and relative molar mass of each crystalline product are: Compound Formula Molar Mass EDTA ci OH1 6N208 292.2 NazEDTAe2H20 CioHiaN2OioNaz 31 2.2 Na4EDTA02H20 C 1 0H16N201 oNa4 416.2 2.2
13、 Hazardous Properties. The Na4 EDTA solution product generally contains excess caustic and can cause permanent damage to the eyes. Contact of solutions of EDTA salts with aluminum can generate hydrogen. 2.3 Handling and Storage. All compounds shall be stored in closed containers at room temperature.
14、 3. Summary of Requirements A summary of requirements for EDTA compounds shall be as given in Table 1. 4. Reagents, Materials, and Glassware 4.1 Reagents 4.1.1 Reagents shall be handled in conformity with health and safety precautions, as shown on containers or as given in other sources of such info
15、rmation, Proper labeling of prepared reagents includes name, date of preparation, expiration date, restandardization date, and adequate health and safety precautions. The dispo- sal of reagents and all materials shall conform to appli- cable environmental regulations. ANSI PH4.185-1987 e 4.1.2 Reage
16、ntsysed in the test procedure shall be certified reagent-grade chemicals and shall meet the specifications given in Reagertt Chemicals published by the American Chemical Society (ACS) in 1981 or shall be chemicals of a purity acceptable for the analysis. The acids and ammonium solutions referred to
17、in all the instructions shall be of full strength unless dilution is specified. Dilution is specified in terms of molarity, M, when standardization is required. The number of significant figures to which molarity is known shall be ,sufficient to ensure that the reagent does not limit the reliability
18、 of the test method. When dilution is indi- cated as (1 t X), it means that one volume of the speci- fied reagent is added to X volumes of distilled water. 4.2 Water. Whenever water is specified in the test pro- cedure, only distilled water or water of at least equal purity shall be used. 4.3 Glassw
19、are. All glassware subject to heating shall be of heat-resistant glass, for example, Pyrex or equiva- lent. . I i 5. Test The tests described in Sections 6 through 11 shall be made to determine whether the test samples meet the purity requirements listed in Section 3. Tests shall be made on samples
20、in their “as received” condition. In the last several years, there have been great im- provements in instrumentation for various analyses. Where such techniques have the equivalent precision and bias, they may be used in place of the tests de- scribed in this standard. 6, Assa y See Table 1. 6.1 Rea
21、gents 6.1.1 PAN Indicator. Dissolve 0.050 gram of l(2- pyridylazo) 2-naphthol in 75 mL of methanl., Add 25 mL of water, and mix well. J Available from American Chemical Society, 1155 Sixteenth Street, NiV, Washington, DC 20036. b DANGER: May be fatal or cause blindness if swallowed. Harmful if inhal
22、ed. If swallowed, induce vomiting. Obtain med- ical attention immediately. 3DANGER: Flammable. Keep away from heat, sparks, and flame, Use with adequate ventilation. I Copyright American National Standards Institute Provided by IHS under license with ANSI Licensee=USN Ship Repair Facility Yokosuka/9
23、961031100 Not for Resale, 05/09/2007 01:34:14 MDTNo reproduction or networking permitted without license from IHS -,-,- A N S I PH4.385 87 H 0724350 OOL3267 7 W Page 3 of 5 pages Table 1 Summary of Requirements K4 EDTA Na4EDTA (“&EDTA Property EDTA Nap EDTA*2H2 O Na4 EDTA*2H2 O Solution Solution Sol
24、ution Assay, minimum 99% (m/m) 98% (mim) 98% (m/m) 45% (m/m) 39% (m/m) 44% (m/m) .p pH at 25C 2.5 -2.9 4.0-5.3 10.0-11.0 No No 4.6-5.2 (saturated) requirement requirement applicable applicable applicable as KOH as NaOH applicable I Free alkali Not Not Not 2.1% max 1.5% max Not Heavy metals 0.001% (m
25、/m) 0.001% (m/m) 0.002% (m/m) 0.005% (m/m) 0.005% (m/m) 0.005% (m/m) (as Pb) max max max max max max Iron (Fe) 0.001% (mlm) 0.001% (m/m) 0.001% (m/m) 0.001% (m/m) 0.001% (m/m) .% (m/m) max max max max max max NOTE: m/m = mass per mass (weight per weight) 6.1.2 Sodium Acetate Buffer (approximate pH 4
26、.7). Dissolve 34 grams of sodium acetate trihydrate in 500 mL of water, and add 15 mL of glacial acetic aid.4, 6.1.3 Cupric Nitrate, 0.1 Molar Solution. Dissolve 24.2 grams of cupric nitrate 2-1/2 hydrate crystals in 700 mL of water, Dilute to 1 liter in a volumetric flask. 6.1.3.1 Standardization.
27、Weigh, to the nearest 0.0001 gram, 0.5 gram of EDTA, 100.00% (J. T. Baker, ULTREX EDTA, or equivalent), into a 250-mL beaker. Add 150 mL of water and 1 mL of sodium hydroxide4 solution (250 g/L). Stir until dissolved. Add 25 mL of sodium acetate buffer (6.1.2). Adjust the pH to 4.5- 5.5 with glacial
28、 acetic acid,“,5 or sodium hydroxide4 solution (250 g/L). Heat to 95OC. Add 1 mL of PAN indicator (6.1 .i). While hot, titrate with cupric nitrate (6.1.3) to a blue-green endpoint. (weight in grams of EDTA) (3.422) mL of cupric nitrate = molarity of cupric nitrate 6,2 Apparatus, In addition to ordin
29、ary laboratory equipment, a 50-mL-capacity buret shall be used 6.3 Procedure. Weigh, to the nearest 0.0001 gram, the required sample weight shown in Table 2 for the spe- cific EDTA compound into a 250-mL beaker. Add DANGER: Corrosive, causes burns. Avoid contact with eyes, skin, and clothing. Wash t
30、horoughly after handling, In case of contact. flush eves and skin with water. Obtain medical atten- z tion immediateiy. open flame. Use with adequate ventilation. DANGER: Combustible, Keep away from heat, sparks, and 150 mL of water and 1 mL of sodium hydroxide4 solu- tion (250 g/L). Stir until diss
31、olved. Add 25 mL of sodi- um acetate buffer (6.1.2). Adjust the pH to 4.5-5.5 with acetic 95OC. Add 1 mL of PAN indicator (6.1.1). While hot, titrate with cupric nitrate to a permanent blue-green endpoint. (mL of cupric nitrate) (molarity cupric nitrate) (A) grams of sample = EDTA compound where (A)
32、 is selected from Table 2 Table 2 Calculation Factors or sodium hydroxide? Heat to Sample Weight Required Compound mams) (A) 29.23 EDTA NapEDTAe2H20 0.6 10.1 37.23 Na4EDTA02H20 0.7 1 0.1 41.62 Na4EDTA solution 1.7 10.1 38 .O2 K4EDTA solution 1.7 1 0.1 44.46 32.63 (“&EDTA solution 0.5 1 0.1 1.7 1 0.1
33、 7. pH See Table 1. Weigh 5.0 grams of the sample into a 250-mL beaker, and add 100 mL of water. Heat to 70C, stir, cool to 25OC (disregard undissolved material), and measure the pH of the solution using a standardized pH meter equipped with a glass-calomel electrode system. ANSI PH4.185-1987 Copyri
34、ght American National Standards Institute Provided by IHS under license with ANSI Licensee=USN Ship Repair Facility Yokosuka/9961031100 Not for Resale, 05/09/2007 01:34:14 MDTNo reproduction or networking permitted without license from IHS -,-,- - A N S I PH4.185 87 W O724350 00312bB 7 W Page 4 of 5
35、 pages 8. Free Aikali 8.1 Reagents 8.1.1 Calcium Chloride, 0.5 Molar Standard Solu- tion. Dissolve 50.00 grams of chelometric standard calcium carbonate (assay 99.95% - 100.5%) in 300 mL of water by slowly adding 86 mL of hydrochloric a i d , to dissolve the calcium carbonate. Heat to boil- ing to r
36、emove carbon dioxide, cool to room tempera- ture, transfer to a I-liter volumetric flask, and dilute to the mark with water. 8.1.2 Sodium Hydroxide 0.1 Molar Solution (4 g/L). An analyzed reagent solution is recommended. This is commercially available from several vendors. 8.1.3 Sulfuric Acid, 0.05
37、Molar Solution (4.9 g/L). An analyzed reagent solution is recommended. This is commercially available from several vendors. ? 8.2 Apparatus. See 6.2. 8.3 Procedure. To a 250-mL beaker containing 25 mL of the calcium chloride standard solution (8.1.1) add 25 mL of water, Add 3 to 6 drops of phenolpht
38、halein indicator solution, and then add 0.1 M sodium hydrox- ide4 (8.1.2) until the solution becomes faintly pink. Add a few drops of 0.05 M sulfuric acid4 (8.1.3) until the color is just discharged, Weigh 6.0 grams of K4EDTA or Na4EDTA solution in a 250-mL conical flask, add 50 mL of water and the
39、neutralized calcium chloride solution prepared above, and titrate with 0.05 M sulfuric acid4 to a faint pink endpoint. (mL H2S04) (M H2 SO4) (8) weight of sample, in grams = percent free alkali as NaOH (mL H2 SO4) (M H2 SO4) (1 1.2) weight of sample, in grams = percent free alkali as KOH 9. Heavy Me
40、tais (as Pb) See Table 1. NOTE: Although this procedure is written to include a l i the compounds listed in the Scope, refer to Table 3 for details appropriate to the specific compound being tested. Table 3 Volume of Hydrochloric Acid and of Aliquot Hydrochloric Acid Aliquot Sample ( m u mL) EDTA 0,
41、5 20 Na2EDTAo2H20 3.0 20 Na4EDTAo2H20 4.5 10 Na4EDTA solution 2.5 4 K4EDTA solution 2.5 4 (“&EDTA solution 2.5 4 9.1 Reagents Dissolve 1.8 grams of lead acetate trihydrate b(C2H302)2*3H20 in water, Dilute to 1 liter with water, and mix well. Pipet a IO-mL aliquot into a 1-liter volumetric flask, dil
42、ute to the mark with water, and mix well. 9.1.2 p-Nitrophenol Indicator Solution, Weigh 2.5 grams of p-nitrophenol, and dissolve in 1 liter of water. 9.1.3 iron Standard (1 mL = 0.01 mg Fe). Dissolve 0.70 gram of ferrous ammonium sulfate hexahydrate Fe(NH4)2(S04)2*6H20 in 50 mL of water, and add 20
43、mL of dilute sulfuric acid4 (1 t 15). Dilute to 1 liter with water, and mix well, Dilute a IO-mL aliquot of this solution to 100 mL with water, and mix well. sodium sulfide, nonahydrate6 (Na2S*9H20) in 100 mL of water. 9.1.1 Heavy Metals Standard (i mL = 0.01 mg Pb). 9.1.4 Sodium Sulfide Solution. D
44、issolve 5 grams of 9.2 Apparatus. Two matched Nessler color comparison cylinders, of 50-mL capacity, shall be used. 9.3 Procedure. Incinerate 5.0 grams of the powdered sample (or evaporate to dryness and incinerate 5.0 grams of solution) in a platinum crucible, and then ignite the residue at 6OO0C f
45、 25C for 4 hours. After cooling, dissolve the residue in 2 mL of water plus the volume of hydrochloric a i d , shown in Table 3. Warm the solution if necessary to dissolve the residue, and transfer the solution with washing to a 100-mL beaker. Pipet 5.0 mL of the Heavy Metals Standard (9.1 .i) into
46、a second 100-mL beaker containing 20 mL of water. Pipet 5.0 mL of Iron Standard (9.1.3) into a third 100-mL beaker containing 200 mL of water. Treat the two standards and the sample solu- tion as follows: Add two drops of p-nitrophenol indi- cator (9.1,2), and then add dilute ammonium hydrox- ide6,
47、(i t 9), dropwise, until the solution turns yellow. Add dilute hydrochloric a i d , (1 t 99), drop- wise, until the solution becomes colorless, and then 6DANGER: Harmful if inhaled. Avoid breathing dust, vapor, mist, or gas. Use only with adequate ventilation. If inhaled, move to fresh air. Obtain m
48、edical attention immediately. WARNING: Avoid contact with eyes, skin, and clothing. Wash thoroughly after handling, In case of contact, flush eyes and skin with water. Obtain medial attention immediately. ANSI PH4.185-1987 Copyright American National Standards Institute Provided by IHS under license
49、 with ANSI Licensee=USN Ship Repair Facility Yokosuka/9961031100 Not for Resale, 05/09/2007 01:34:14 MDTNo reproduction or networking permitted without license from IHS -,-,- - _ _ _ _ _ ANSI P H 4 - 3 4 5 87 0724350 OOi3269 O Page 5 of 5 pages add O S mL excess. Warm on a steam bath for 10 min- utes. Cool, dilute to 50 mL with water, and mix well. To a 20-mL aliquot of this so