1、ANWNAPM IT4.155-1981 (Rl996) Reatfination and redeslgnation of ANSI PH4.155-1981 (R1987) ReWn of ANSI PH4.155-1974 f American National Standard 7 for Photography (Chemicals) - Aluminum Sulfate Solution Secretariat National Association of Photographic Manufacturers, Inc J Approved January 16, 1981 Re
2、affirmed July 16, 1996 Page 1 of 3 pages Foreword (This Forerord is not a part of Amencan National Standard Specification for Photographic Grade Aluminum Sulfate Solu- tion, ANSI PH4 155-1981.) This standard is one of a series that establislies the inin- imum criteria of purity for clieniicals used
3、in processing photographic iiiaterials However. if the purity of a coniirionly available grade of chernical cucceds the iiiiii- iinuin criteria arid if there is no ecoiioini: peiiliity in its use, the purity requireiiieiiis have heeii st to take ad- vantage of the higher quality iiiacri;lI. Although
4、 rlie ultiiiiate criterion for suitability ofa photogi-apliic grade cliriiiical is Its uccessful perfoi- inance iii an appropriate photographic use test. the shorter. inore ecoiioiiiical tests described herein are generally adequate. This standard is a revision of.4iiirricari Natioiial Standard Spec
5、iBcation for Photographic Grade Aluiiii- num Sulfate Solution. AI2(SO4 )3. ASSI Pii4 155- 1974. In this latest revision, precautions have beeii edi- torially corrected. and Section I has been expanded 1. Scope This standard establishes criteria for the purity of photographic grade aluniiiiurii sulfa
6、te solution and de- scribes the tests to be used to deteriiiirie the purity. 2. General Infomation 2.1 Physical Appearance. Aluitiiriiiiii sulfate solution is usually clear and colorless. The iiiolecular weight ot anhydrous aluiiiiriuiii sulfate is 343. i 5 2.2 Hazardous Properties. Aluniinuni sulfa
7、te solution is very low in toxicity and is noncoiiibustible. 2.3 Handling and Storage. No special precautions are required. 3. Summary of Requirements Assay as Alz(S04), by weight Specific Gravity (at ?O/O“O. Appearmcr of Solutioii Free .4lkaliiiity and Free Acidity. 18.1% max 76.87 inin I 333 iiiax
8、 i .3 14 niin To pass test 0.70,+ iiiax as 0. 10% iiiax as H2 so4 0.0 17 inax .A12 0, Heiivy Metals (3s Pb ) Iron ( Fe) 0.0055 rnax 4. Test Sainples. Reagents, Solutions, aiid Hazards 4.1 Sainples. Tests shall he iiiade on saiiiples in their “as received“ condition 4.2 Punty of Reagents meet the spe
9、cifications given in Reagent Chemicals, published by the American Cheniical Society in 1974, wherever such specifications have been established. If no American Cheniical Society specification exists, the 4.2.1 Reagents used in the test procedures shall Available from American Cheinical Society, 1155
10、 Sixteenth Street, NW, Washington, D C. 20036. CAUTION NOTICE This American National Standard may be revised or withdrawn at any time The procedures of the American National Standards Insti- tute require that action be taken to reaffirm. revise. or withdraw this standard no later than five years fro
11、m the date of publication Purchasers of American National Standards may receive current information on all standards by calling or writing the American National Standards Institute Printed in USA COpyrQht O 1981 by American National Standards Institute, 11 West 42nd Street, New York, N.Y. 10036 Page
12、 2 of 3 pages 5. Test Procedures i. Specific Gravit! (at zo OOC) ( 1.333 11i3xi11iuiii. 1 3 14 iiiiiiiiiiiiiii I 8. Appearance of Soliitioii (To pass fest) ANSVNAPM lT4.155-1981 (R199) Page 3 of 3 pages 9. Free Alkalinity and Free Acidity (0.2maximumasA1203,0.1070maximumasH2S04) Dissolve 3 grains 2
13、0. i grairi of sodiuiii 50 niL of hot water in a 125-niL conical flask and add 3 drops of 1 0% phenolphthalein (10 g/L alcohol solu- tion). Carefully neutralize. using 0. 1 IV sodium hydrox- ide4 or 0.1 N hydrochloric aid. To 5.0 grams 50.1 graiii of sample in a 250-iiiL conical flask, add 3 boiling
14、 chips, 10 iiiL of water, and 25.0 iiiL of 0. i N sulfuric acid.4 Heat to boiling. Allow the solution to cool to room teiiiperature in a water bath. Add the cool. neu- tralized sodiuiii fluoride solutioi to the sample solu- tion and niix well. Titrate with 0. 1 N sodiuiii hydrox- than (iiiL H2 SO4 X
15、 N), calculate free alkalinity: in . ide4 to a pale pink color. If (iiiL NaOH X N) is less I (mL H2 SO4 X N) - (iriL NaOH X iV) (1 7) - sample weight in grains = percent A1203 If (mL H2 SO4 X N is less than (iiiL NaOH X N), cal- culate free acidity. (niL NaOH X N) - (inL H2 SO4 X N) (4.9) sample wei
16、ght in granis = percent H2 SO4 10. Heavy Metals (0.01% maximum as Pb) 10.1 Heavy Metals Standard (1 mL = 0.01 mg Pb). Dissolve i .8 gram _+ 0.1 gram of lead acetate3 Pb(C2 H3O2 j2 .3H20 in water. Dilute to i liter with water and mix well. Transfer a 10-iiiL aliquot to a I-liter volumetric flask. dil
17、ute with water to the mark, and inix well. 10.2 Iron Standard (i mL = 0.01 ing Fe), Dissolve 0.70 grain * 0.05 grani of ferrous aniiiioiiiuiii sulfate Fe(NH4)2(S04)2-6H20 in 50 iiiL ofwater in a 1-liter voluiiietric flask. Add 20 iiiL of dilute sulfuric acid4 (i + 15). Dilute to the I-liter iiiark w
18、ith water and mix well Dilute a 10-iiiL aliquot of this solution to i00 inL with water in a 100-iriL voluinetric flask and mix well. I _ CAUTION: Avoid contact with eyes, skin, and clothing. Wash thoroughly after handling. In case of contact, flush eyes and skin with water. Obtain medical attention
19、immediately. CAUTION: Harmful if swallowed. Wash thoroughly after handling. If swallowed, induce vomiting. Obtain medical atten- tion immediately. O 10.3 Procedure. Dilute 1 .O graiii 2 0. i gram (about 0.8 iiiL) of the sairiple with approximately 25 mL of water in a 100-iriL beaker Pipet 10.0 niL o
20、fthe Heavy Metals Standard into a second 100-iiiL beaker containing 20 niL of water. Pipet 5 iriL of the Iron Standard into a third 100-niL beaker containing 20 niL of water. Treat both standards and the saiiiple solution as follows. Add 2 drops ofp-nitroplienol indicator (2.5 g/L aqueous solution)
21、and then add dilute hydrochloric acidzT3 (i + 5), dropwise, until the solution becorries colorless, then add one drop excess. Warin on a steam bath for 10 minutes. cool. aiid dilute to 50 mL with water. To 20-mL aliquots of both the treated Heavy Metals Stan- dard and the treated saiiiple solution (
22、save the treated Iron Standard aiid the balance of the treated sample solution for the iron test in Section 1 l), add 5 iiiL of hydrogen sulfide water,7 dilute to 50 riiL with water, and transfer to Nessler color comparison tubes. Any color produced in the treated saiiiple solution shall not exceed
23、that produced in the treated Heavy Metals Stan- dard solution. 11. Iron (0.005% maximum Fe) 1 1.1 Reagents 11.1.1 pH 5 Acetate Buffer. Add 23 graiiis of anhy- drous sodiuiii acetate to 60 iiiL of dilute acetic acid4 (1 + 8) and dilute to 1 liter with water. Adjust the final pH of the solution to 5 O
24、 f 0. 1 at 21C with dilute acetic acid4 (1 + 8) or sodiuiii hydroxide solution4 11.1.2 1 ,lo-Phenanthroline (o-Phenanthroline) Mixture. Thoroughly imx equal volunies of ai1 aqueous solution of 1 ,lO-pIienaiithroline (1 g/L), an aqueous solution of hydroxylaiiiine hydrochloride2 ( 100 g/L). and pH 5
25、acetate buffer. 11.2 Procedure. Traiisfer a 10-iiiL aliquot of the solu- tion coiitaining the Iroii Staiidard to a 100-iiiL beaker. To a second 100-iiiL beaker containing 10 iiiL of water add a 10-iiiL aliquot of the sample solution prepared in 10.3. Add 5 inL of the 1.10-pheiiaiitliroliiie mixture
26、to each beaker, mix well. aiid let stand for 10 iiiinutes. Dilute to 50 iiiL with water. mix well. aiid transfer to Nessler color coiiiparisoii tubes. Any color produced in the treated saiiiple solutioii shall not exceed that pro- duced in the treated Iroii Staridard solution ( 100 dL). DANGER: Harmful if inhaled. Avoid breathing dust, vapor, mist, and gas. Use only with adequate ventilation. If inhaled, move to fresh air. Obtain niedical attention immediately. ANSUNAPM IT4.155-1981 (R1996) , I
