1、ANSVNAPM 114.177-1983 (RlS96) Reaffimation and redesignation of ANSI PH4.1TI-1983 (R1987) Revision of ANSI PH4.177-1972 American National Standard . I for Photography (Chemicals) - Sodium Thiocyanate Crystals and Solution (50%) Approved May 5, 1983 Reatfirmed July 16, 1996 Secretariat: National Asso
2、ciation of Photographic Manufacturers, Inc I Foreword (This Foreword is not part of American National Standard PH4.177-1983.) This standard is one of a series that establishes criteria of purit) for chemicals used in processing photographic nia terials Although the ultiiriate criterion for suitabili
3、ty of a photographic grade chemical is its successtul perfor- mance in an appropriate photographic use test. the shorter more economical tests described herein are gen- e rally adequate. This standard Is a revision of American Sacional Standard Specifcation for Photographic Grade Sodium Thioc) anate
4、. NaSCN. ANSI PH3. I 77-1 972 In this latest revision. iiiinor changes have been made in the expressions of solution concentrations and calculations. precautions have been added. and the section on gen- eral intorniation has been expanded. Also. this standard is no1 molecular weight of 8 1 .O8 sligl
5、itly taii colored liquid. 2.2 Hazardous Properties. Sodium thiocyanate is inod- erately toxic and can act as an allergen and skin irritant. 2.3 Handling and Storage. Sodium thiocyanate should be kept away roiri open tlaines Exposure to open 2.1.1 Solid sodium thiocyanate is in the foriii of 2.1.2 So
6、diuiii thiocyanate solution is a colorless to Page 2 of 5 pages flames may generate poisonous hydrogen sulfide and hydrogen cyanide gases. 3. Suiiiinary of Requirements Cr1.s fall 111 e 3 5 f: Il19.X 95 07 iiiin o 3; Illax 0.2; IllJX o 0011 171ax 0.0087 inax Solir tiriri 50 O? 111111 o 257 i11a.y 0.
7、0005:; inax o 01; max o 004; ill ;ty 65+05 1305-1 320 So turbidity 50 .4PHAi m.i 1 5; Illax 0.029 i113X - . - 0 17 Ill3X 4. Test Saiiipies. Reagents. Solutions. and H azar ds 4.2.2 Wherever water is specified in the test proce- dures, only distilled or deionized water shall be used. 4.3 Strength of
8、Solutions 4.3.1 Acids and ammonium hydroxide shall be fI1 strength uiiless otherwise specified 4.3.2 Wheri a standardized solution IS required. it ioncenrraiion is expressed as norniality. A. The iiuni- ber of significant figures 10 which the norrnalit is known shall be siiffcient ICI ensure that th
9、e reagent does not tiinit th reii.ibilit) i the lest irieihod. its coiicentration is expressed 3s grains per liter (giL) to the appropriate nurnber of significant figures. 4.3.4 Wheri a solution is to be diluted, its diluticn is indicated by (i + X). meaning that one volume of reagent. or concentrat
10、ed solution. is to be diluted with X volumes of water. 4.4 Hazards. Some of the chemicals specified iri the test procedures are caustic. toxic. or otherwise hazai-d- OUS. Specific caution. warning. and danger notices are given in the footnotes but. in addition. the normal pre- cautions required duri
11、ng the performance of any chmi- icai procedure must be exercised at all times 4.3.3 Wheri a standardized solution is not requirzd. 5. Test Procedures The trst procedures described in Sections 6 throuh 19 shall be folloed IO dereriiiine whether the tesr jarriple inssts tti? PUII! requirrnierits liste
12、d III Stc. tiuri 3 in lie 1.iht wer31 jcdrs there hve been great 1111- provenieii ts in ritrinentioii for arious aiiAses Uliere juiti teihniquzs hare the equivalent accuracy and preiision. the, niay be used III place of the test deibed in this standard 6. Volatile Matter at 105C (3.5; maximum) ANSLN
13、APhl IT4.177-1983 (R199b) Page 3 of 5 pages 7. Assay Crystalline Sodium Thiocyanate (NaSCN) (95.0% minimum) Sodium Thiocyanate Solution (50% minimum) Weigh about 3.0 grains of crystallirit sodiuin thiozya- rate. or 6 O grains of sodiuin thiocyanate soltiori. to the nearest O 1 my in a glass-stoppere
14、d weighing bottle Transfer with washiiig to a 500-iiiL volumetric flask. dilute t3 the inark with water. stopper the flask. and mix thoroughly b), inverting the flask 3 or 4 tiiiies to ensurt. uiiiforiii soiution Pipet a SOL aiquot. into a 500-nil glass-stoppered Erlenmeyer flask. Add i5 in1 of benq
15、.1 alcoho14.5 and pipet 50 mL of O i A silver nitrate4 into the sample soltion. with con- stant shaking of the Erlenmeyer flask. Add i niL of nitric acid6 and titrate the excess silver nitrate with O Ill ainmonium thiocyanate3. using I inL of a saturated aqueous solution of ferric ainmoniuin sulfate
16、 as indicator Shake viyorously after the addition of each drop near the end point Take the end point as the first permanent perceptible peach tinge Percent NaSCN - (sO.OOl WAgN03 _ i-(mL NH,SCN) (NNH4SCN) grams of sample X 81.08 - 8. Alcohol - Insoluble Matter Weigh to the nearest milligram 5.0 grai
17、ns of the crys- talline 75 ml of ethyl alcohol to the sample in the beaker. Cover and place beaker on a steam bath for i hour. Filter the hot solution through a tared sintered-bottom crucible of medium porosity and wash with three 10 mL portions of hot (about 7OoC i ethyl alcohol.* Dry crucible at 1
18、05C for 4 hours. cool in a desciccator, and reweigh. The residue shall not exceed O 075 gram. in a tared 250-mL beaker. Add about WARNING: Harmful if inhaled. Avoid breathng dust, vapor, mist. or gas. Use only with adequate ventilation. If inhaled, move to fresh au. Obtam medical attention immediate
19、ly. DANGER: Corrosive, causes burns. Avoid contact with eyes, skin, and clothng Wash thoroughly after handling. in case of contact, flush eyes and skin with water. Obtain medical atten- tion immediately. DANGER: Avoid contact with eyes, skin, and clothing. Wash thoroughly after handling. in case of
20、contact, flush eyes and skin with water. Obtain medical attention immediately. DANGER: Flammable Keep away from heat, sparks, and open flame. Use with adequate ventdation. 9. Alkalinity (0.375 maximum as NaOH) Dissolve 5 O grams f O 1 gram of the crystalline sam- in 50 niL of carbon-dioxide-free wat
21、er in a 350-nil Erlenmeyer flask. Add 3 drops of phenolphtha- lein indicator (O 1 gram per 100 niL of alcohol) to the dissolved sample Titrate with 0.1 N hydrochloric aid. to the di5appearance of the pink color percerit T$ OH = (ml - HCI) (A HCI) (4.0) ,a grams of sample 10. Total Ammonia (0.255 max
22、imum as NH3) Weigh 10.0 grains f O. i gram of well-shaken 50% solu- tion in a glass-stoppered weighing bottle. Trans- fer with washing to a 500-mL Kjeldahl-type flask contain- ing about 100 nil of water and then connect flask to a spra! trap and condenser Pipet 25.0 mL of 0.1 N hydrochloric acid4* i
23、nto a ?SO-mL Erlenmeyer flask and place the tip of the condenser beneath this solu- tion. Add 20 inL of aqueous sodium hydroxide solu- ion6 (100 g/L) to the sample3y4 in the Kjeldahl-type flask, immediately stopper. and distill for one-half hour. Remove the receiving flask (250-mL Erlenmeyer flask i
24、 from the condenser and add 2 drops of phenolphthalein indicator to the solution in the receiving flask. Titrate to the pink endpoint with 0.1 N sodium hydroxide.6 Percent NH3 - (mL HCI) (N HCI) - (mL Nag (N NaOH) ,7 grams of sample 11. Halides Crystalline Sodium Thiocyanate (0.2% maximum as Ci) Sod
25、ium Thiocyanate Solution (0.1% maximum as Ci) 11.1 Halide Standard (1 mL = O. 1 mg CI). Dissolve 0.835 gram of sodium chloride in some water in a 1- liter volumetric flask. Dilute to the mark with water and mix well. Transfer a 100-niL aliquot of this solu- tion to a 500-inL volunietric flask. Dilut
26、e with water to the mark and mix well. 11.2 Procedure. Dissolve i .O gram f 0.01 gram of crys- talline arnple. in 20 mL of water in a 135-mL conical flask. Into a second i 3s-niL conical flask. pipet 20 nil of the or 3.0 grams 2 0.01 gram of solution ANSUNAPM lT4.177-1983 (R1996) Page 4 of 5 papes H
27、alide Standard and add 10 iiiL oi water Treat the stand:ird and the sample soltion. in the sanie nian- ner Iri clieiiiicl JLIIIIL hood. sloaly add 10 iiiL of sulfuric acid4 ( 1 + 2) aiid. with constant swirling. add 7 iiii of 20 percent li! dropii peroxide NOTF Storc ?O perLcnt ti! drc1gc.n peroxide
28、 in reiriper3tor frcc from eIi1) oudized nl.tcri.lc and chcmiCdl fUillCF Isr c3itioi1s1 Fi! drqcii pcroidc6 is a pouerful oyi- dnt niateril liuid LOII.IC( 4illl skin aiid ejes In Lase ofonct. fliisi nith uater Iri this re3itioii t genrr.ies i! iiidc Juiiie uhiih 3rc poiwiious Coiicen- trare 10 pproi
29、iiiatcl 20 niL b boiling in a well- wnti13ted Iiood Add 20 iiiL of “Jter aiid again evapo- rdtc ti) 20 iiiL Cool aiid dilute to 100 niL. To 3 20-iiiL aliquot. add 1 mL cit.tiitrI mix. then Add O 2 niL (approxiiiiatcly 4 drciphi ot aqueous silver nitrate solu- 11011 ( 100 cLi. nii vc.ll. and transfer
30、 to Nessler color coiiiparison tubes An) turbidit! produced in the saili- ple scdutioii sliall not exceed that produced iii the t re 3 t c d Halid e St an dd r d sol II ti o11 12. Sulfidiiig Compounds Crystalline Sodium Thiocyanate (0.001% maximum as S) Sodium Thiocyanate Solution (0.000% maximum as
31、 S) NOTE In addition to the sulfide ion, this procedure measures sulfur linkages UI compounds such as thiourea 12.1 Sulfiding Compounds Standard (i mL = 0.05 mg S). This Toluiioii must be treshly prepared Dissolve O 75 graiii ? O O2 gram ofsodiuiii sultide rionahydrate (Ka2S*9H20) in a I-liter volui
32、iietric flask of freshly boiled and cooled water. Dilute a 35-inL aliquot of this solution to 50 rnL in a voluiiietric flask and inix well. 12.2 Procedure. Dissolve 5.0 graiiis ? O I gram crystal- line saniple3 or 10.0 graiiis ? O 1 grain of the solution aniple. in SO inL of water in a 2SO-niL beake
33、r Pipet 1 mL of the Sulfiding Compounds Standard into an- other 3O-mL beaher containing 50 iiiL of water Treat the standard and the sample solutions in the sanie manner. With vigorous stirring. add 75 inL of a freshly prepared solution consisting of 10 inL of silver nitrate solution4 (100 giL) and 1
34、5 iiiL ot aiiiinoniuiii hydrox- ide 4.s Cover with watch glasses aiid heat on a steam bath for IO minute5 Any dark precipitatc 01 color pro- duced in tlic sample solution shall not exceed that pro- duced in the standard (CAUTION Dispose of all reagents and test solutions and rinse apparatuc immcdiat
35、ely. An euplotrve compound may be formed on standing.) 13. Heavy Metals Crystalline Sodium Thiocyanate (0.02% maximum as Pb) Sodium Thiocyanate Solution (0.01% as Pb) 13.1 Heavy Metals Standard (1 mL = 0.01 mg Pb). Dissolve 1.8 grams ? 0.1 grani of lead acetate trihy- drate Pb(C, H302 ).3H20 in wate
36、r. dilute with water to 1 liter in a volumetric flask. and n11x well Pipet a IO-iiiL aliquot of this solution into a I-liter volunietric flask. dilute with water to mark. and mix well 13.2 Procedure. Dissolv. 2 5 granis ?0.0001 eram of the crystallinc ariiple. or 5 O grams f O 0001 grain of the solu
37、tion saniple3. in water and dilute Hith water to 30 rnL in a volumetric flask Pipet 75 mL o! this solution into a 115-mL conical flask and pipet 5 inL of the Heq. Metals Standard into a second 125. rnL conical flask. Treat the standard and the sample olutions in the sanie manner Add I drop ot p-nitr
38、ophenol indicator (2 5 g L aqueous solution) Add hydrochloric aid. (1 + 99) dropwise until the solution becomes colorless. and then add O 5 niL excess Add 5 ml OJ hydrogen sulfide water.9 dilute to 50 rriL with water. niix well. and transfer t Kessler color coiiiparisori tubes Any color produced in
39、the sarnplc solution shall not exceed that produced in the treated Heavy Metals Standard solution 14. Iron Crystalline Sodium Thiocyanate (0.008% maximum Fe) Sodium Thiocyanate Solution (O.04% maximum Fe) 14.1 Reagents anhydrous sodium acetate in 60 niL of acetic acid6 ( 1 + 6) and dilute with water
40、 to 1 liter. Adjust the final pH of the solution io 5 O ? 0 I with acetic acid6 (i + 8). or with sodium hydroxide solution6 (100 g;L) 14. i .2 1 .IO-Phenanthrohe (o-Phenanthroline) Mixture. Thoroughly mix equal volumes of an aqueoLs solution of .IO-plienanthrolirie (1 g:L). a solution of hydroxylami
41、ne hydrochloride4 ( 100 g/L). and pH 5 acetate bu fter 14.2 Iron Standard (1 rnL = 0.01 rng Fe). Dis- solve O 70 gram of ferrous aiiimoniuri sulfate IFe(NH4)2(S04 )2.6H20 in 50 mL of water and ad3 20 mL of dilute sulfuric acid4 ( 1 + 15) Transfer to a 14.1.1 pH 5 Acetate Buffer. Dissolve 23 grams of
42、 - “DANCER: Harmful if inhaled. Avoid breathg dust, vapoi mist, or pas. Use only with ddequate ventilation. If inhaled. move to fresh air. btdin medical attention immediatel). ANSUNAPM IT4.177-1983 (R1996) Page 5 of 5 pages I-liter volumetric flask, dilute to the mark with water, and nib. well. Pipe
43、t a IO-mL aliquot of this solution in a 100-mL volumetric flask, dilute to the mark with water. and nux well. n 14.3 Procedure. Dissolve 12.5 grams t 0.1 gram of the crystalline arnple. or 25.0 grams f 0.1 gram of the solution aniple. in 50 mL of water and add 1 mL of hydrochloric acid.4* Warm for 3
44、0 minutes on a stem bath. cool. filter. and dilute to IO0 mL. To S-mL aliquots of the Iron Standard and the sample solutions in 100-iiiL beakers. add 5 niL of 1.10-phenanthroline mixture. mix well, and let stand for IO minutes. Dilute to SO mL with water, mix well, and transfer to Nessler color comp
45、arison tubes. Any color produced in the sample solution shall not exceed that produced in the treated Iron Standard solution. I 15. pH (6.5 t 0.5 at 2OoC for Sodium Thiocyanate Solution) Determine the pH of the solution ample. at 20C using a suitable pH meter See American National Stan- dard Method
46、for the Determination of pH of Photo- graphic Processing Solutions. and Specifications for pH Meters Used to Measure pH of Photographic Pro- cessing Solutions, ANSI PH4.36- 1978 a 16. Specific Gravity 1.305 to 1.320 (2O/2O0C for Sodium Thiocyanate Solution Determine the specific gravity of the solut
47、ion sam- ple3.4 at 20C by means of a pycnometer, a 5-mL specific gravity laboratory type used with a precision analytical balance, or by any other equally accurate means. 17. Appearance of Sodium Thiocyanate Solution Sample shall be a clear solution with no turbidity. 18. Color (APHA) of Sodium Thio
48、cyanate Solu tion 18.1 Preparation of APHA Color Standard. Dissolve 1.245 grams of potassium chloroplatinate (K,PtCI,) and 1 .O gram crystallized cobaltous chloride (CoCI2 -6H20) in water with 100 mL concentrated hydro- chloric acid4. in a I-liter volumetric flask. Dilute to the 1 liter mark with wa
49、ter. Stopper flask. mix well by inverting flask several times. Dilute S mL of this solution to SO mL with water in a Nessler color com- parison tube. This resulting solution has an APHA color of 50. 18.2 Procedure. Compare 50 mL of the sample with SO mL of a potassium-cobalt standard, APHA of SO. in Nessler color comparison tubes. The color of the sample must be equal to or less than the color of the APHA color standard.
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