1、ANSVNAPM lT4.231-1982 (R1996) Reaffirmation and redesignation of ANSI PH4.231-1982(R1987) Revision of ANSI PH4 231-1976 7 American National Standard for Photography (Chemicals) - Sodium Metaborate Octahydrate Secretariat: National Association of Photographic Manufacturers, Inc Approved February 26,
2、1982 Reaffirmed July 16, 1996 Foreword (This Foreword is not a part of American National Standard Specification for Photographic Grade Sodium Metaborate Octahydrate, ANSI PH4.23 1-1982.) This is one of a series of standards that establishes cri- teria of punty for chemicals used in processing photo-
3、 graphic materials. Although the ultimate criterion for suitability of a photographic grade chemical is Its successful use in an appropnate photographic use test. the shorter. more economical tests described herein are generally ade- quate. This standard is a revision of American National Standard S
4、pecification for Photoyaphic Grade Sodium Metaborate Octahydrate. ANSI PH4.23 1-1976. In this latest revision, minor changes in precaution notations have been made and the general format has been up- dated to reflect current procedure. I. Scope This specification establishes criteria for the purity
5、of photographic grade sodium metaborate octahydrate (Na2 B2O4.8H20) and describes the tests to be used to determine the purity. Paee i of 4 paees 2. General Information 2.1 Physical Properties. Sodium metaborate octahy- drate is in the form of white crystals and has ri molecu- lar weight of 375.8. 2
6、.2 Hazardous Properties. This niaterial is not hazard. ous when handled with normal precautions. 2.3 Handling and Storage. Store in tightly closed con- tainers. 3. Summary of Requirements pH (at 75C). Halides (as Ci), Heavy Metals (as Pb) Iron (Fe). Carbonate Reaction to Amnioniricul Appearance of S
7、olution: Silver Nitrate 98.57 min 1 O2 .O5 mas 10.80-1 1.10 o. 1 % max 0.0015 mux 0.0037 11135 To pass test To pass test To pass test An Ainericdn Fidtional Simddrd iniplie a conxmtuc o1 thc ul)tdnti.ill) conccrncd villi it ctpc .inJ proviioiiv. An Aincricdn NdtimJl Stdnddrd I iiitcndcd .I a guide t
8、o did flic nianutactiirtr. flic contumcr. JnJ tlic esncr.il public The eitciicc o.n 4iiicricdn Ndiional st.iii- dard does not in any rccpect preclude anyone. wlictlicr Iic lias approved tlic tdnddrd or not. Iroiii iiiniiiacruring. in3rkciins. piirclidins. r iizing products. proceses. or procedurec n
9、or coniorniing to the tanddrd .mcrii.in N.itionJl Stdiid.ird drc ubJcct i 15 granis of mannitol and 12 drops of phenolphthaleiii indicator (10 g/L in 95% ethanol) to produce ;1 red color. Titrate with standardized 0.5 h: sodium hdrcn- ide3 until the color changes from red to !elloi anil then yellow
10、to a fairit pinh. 7. pH ( 10.80-1 i. i O at 2SC) Dissolve 10 garis i 0.1 eram of the sample in i liter ot water. Deterrnine the pH othissoiition at 25C ? I “C. usins any suitable pH niete? witti .I lw wdiiiiii i011 crroi V) - (mL NH,SCN).1) 0.0355)(100) grams of sample ammonium thioyanate. using sul
11、fide water. dilute to 50 iiiL vitIl water. mi veil. and transfer to Nessler Color Coniparison tubes Ail! color produced in the sample solution shall not excecd that produced in the Heap Metals Standard solution NOTE: Save the Iron Standard solution cind the reniainin: sample solution for the iron te
12、st in 10.2 9. Heavy Metais (0.001% maximum as Pb) 9.1 Heavy Metals Standard (I mL = 0.01 mg Pb). Dissolve 1.8 grams of lead acetate trihydrate4 Pb(C2H302)2 *3H20) in water. transfer to a I-liter volumetric flask. dilute to the mark with water, and mix well. Pipet a IO-mL aliquot of this solution int
13、o a I-liter volumetric flask, dilute to the mark with water, and mix well. 9.2 Iron Standard (I mL = 0.01 mg Fe). Dis- solve 0.70 gram of ferrous ammonium sulfate Fe(NH4)2(S04)2 *6H2 O in 50 mL of water and add 20 mL of sulfuric acid2 (I + 15). Transfer to a 1-liter volumetric flask, dilute to the m
14、ark with water, and mix well. Dilute a IO-mL aliquot of this solution with water to 100 mL in a volumetric flask. and mix well. 9.3 Procedure. Weigh 3.0 grams ? 0.1 gram of the sam- ple into a 100-mL beaker. add 50 mL of water. and heat to dissolve. Pipet 7 mL of the Heavy Metals Stan- dard solution
15、 into a second 100-mL beaker and dilute with SO mL of water. Into a third 100-mL beaker, pipet 6 mL of the Iron Standard and dilute with 50 mL of water. Treat both standard solutions and the sample solution as follows. Add 1 drop of p-nitro- phenol indicator (7.5 g/L aqueous soiution) and then add h
16、ydrochloric (1 + 3). dropwise. until the solution becomes colorless. Add ammonium hydrox- ide2*4 (I + 9), dropwise. until the solution turns yellow. Add hydrochloric aid. (I + 99). dropwise. until the solution becomes colorless, and then add 5 mL excess. Dilute to 80 mL with water and mix well. To 4
17、0-mL aliquots of the Heavy Metais Standard solu- tion and the sample solution. add 5 mL of hydrogen DANGER: Harmful if swallowed. Wash thoroughly after handling. If swallowed, induce vomiting. Obtam medical at- tention immediately. horoughiy after handling. In case of contact, flush eyes and skin wi
18、th water. Obtain medical attention unmediately. DANGER: Avoid contact with eyes, skin, and clothing. Wash 10. Iron (0.00370 maximum Fe) 10.1 Reagents 10.1.1 pH 5 Acetate Buffer. Add 73 grams of anhy- drous sodium acetate to 60 mL of acetic acid3 (I + 8). and dilute to 1 liter. Adjust the final pH of
19、 the solution to 5.0 f 0.1 with acetic acid3 (I + 8) or sodium hydrox- ide solution3 (i00 g/L). 10.1.2 1,lO Phenanthroline Mixture. Thoroughly mix equal parts of an aqueous solution of 1 .IO-phenan- throline (1 g/L), hydroxylamine hydrochloride solu- tion2 (100 g/L), and the pH 5 acetate buffer. 10.
20、2 Procedure. To 40-mL aliquots of the Iron Stan- dard solution and the sample solution prepared in 9.3. add 5 mL of the 1 ,IO-phenanthroline mixture. mix well, and let stand for 10 minutes. Dilute to 50 mL with water, mix well, transfer to Nessler Color Com- parison tubes. and visually compare. Any
21、color pro- duced in the sample solution shall not exceed that produced in the Iron Standard solution. 1 1. Carbonate (To pass test) Acidify SO niL of a cold. saturated aqueous solution of the sample with sulfuric acid2 (1 + 1). There shall be no effervescence. The absence of effervescence indi- cate
22、s no more than approximately 1% carbonate. 12. Reaction to Ammoniacal Silver Nitrate (To pass test) 12.1 Ammoniacal Silver Nitrate Solution. Mix equal volumes of silver nitrate2 (100 g/L) and ammonium hydroxide .2-4 12.2 Procedure. Prepare a blank by adding 5 mL of DANGER: Harmful if inhaled. Avoid
23、breathing dust, vapor, mist, and gas. Use only with adequate ventilation. If inhaled, move to fresh ar. Obtain medical attention immediately. ANSVNAPM lT4.231-1982 (R1996) Page 4 of 4 pages ammonium Iiydroide. to a solution of 1 srmi ? 0.1 gram of the sample in 25 mL of LIL in 3 50-mL Xessler Color
24、Comparison tube. Dissolve I grarii ? 0.1 gram of the sample in ?O mL of uatcr in a 50-niL Kessler Color Coiiiparison tube. cool the solution 10 30C. add 1 O mL of freshly prepared amnioniacal silver nitrate slution. previously cooled to 2OC. and niil well. Allow the sample and blank solutions to sta
25、nd in the dark for 2 minutes at 20C. Compare these solu- tions against a white background. Any color or precip- itate produced in the sample solution shall not exceed that produced in the blank solution. 13. Appearance of Solution (To pass test) A solution containing 30 grams ofthe sanipl? pr.r li1i.r of water shall be clear at the end of 1 hour A sIi$t flocculence ur coloration may be disregarded ANSUNAPM lT4.231-1982 (R1996)
