1、INTERNATIONAL STANDARD ISO 3299 Second ediiion 1994-11-01 Photography - Processing chemicals - Specifications for 1 -phenyl=3=pyrazolidinone Photographie - Produits chimiques de traitement - Spkifications pour Ia ph is the volume, in millilitres, of the sodium thio- sulfate used for the Sample titra
2、tion (7.1.4); is the volume, in millilitres, of the sodium thiosulfate Solution used for the blank titration (7.1.4); is the mass, in grams, of the test Portion; is the conversion factor obtained from the mass of 1 -phenyl-3-pyrazolidinone equivalent to 1 mole of iodine (i.e. 81 ,l) x the conversion
3、 factor for millilitres to litres (i.e. 0,001) x 100 (for percentage). 7.2 Identity tests 7.2.1 Melting Point 7.2.1 .l Specification The melting Point shall A mixed melting Point befrom119”Cto122”C. shall be from 119 OC to 122 “C and shall not be lower than either the Sample or the Standard. 7.2.1.2
4、 Apparatus 7.2.1.2.1 Capillary tube melting Point apparatus, complete with thermometer for the range 100 “C to 200C. 7.2.1.3 Procedure Prepare three capillary tubes containing: a) the Sample to be tested; b) a Sample known to be l-phenyl-3-pyrazolidinone; ISO 3299: 1994(E) c) a finely ground mixture
5、 of a) and b) mixed in equal proportions. Identify the tubes and attach them to the ther- mometer. Heat the apparatus (7.2.1.2.1) to about 100 “C. Insert the thermometer with the samples attached, and thereafter heat at a constant rate of 1 “C/min. Note the melting Point of each Sample as indicated
6、by the first appearance of liquefaction. 7.2.2 lnfrared spectrum 7.2.2.1 Specification The infrared absorption curve shall be essentially the same as that of the reference spectrum (figure 1). This optional recommendation is supplementary to that of 7.2.1. 7.2.2.2 Apparatus 7.2.2.2.1 Test sieve, 63
7、Fm aperture size, con- forming to ISO 565. 7.2.2.2.2 Infrared spectrometer, equipped for the 2 Pm to 16 Fm regions, and accessory equipment for using potassium bromide plates or mineral oil mull. 7.2.2.3 Procedure Grind about 1 g of the Sample to a homogeneous fine powder and prepare a 0,5 % (mlm) m
8、ixture of the Sample in finely ground potassium bromide. Grind together thoroughly to pass through the test sieve (7.2.2.2.1). Prepare a pressed plate of the mixture containing 0,13 g to 0,16 g of the mixture per Square centimetre. Record the infrared spectrum from 2 Pm to 16 Fm. Compare with the re
9、ference spectrum given in figure 1. NOTE 1 As an alternative procedure, the Sample may be ground and dispersed in mineral Oil. It will then be neces- sary to take into account the absorption bands of the Oil. 7.3 Residue after ignition 7.3.1 Specification Maximum residue after ignition shall be 0,lO
10、 % (m/m). 7.3.2 Procedure Determine the percentage residue after ignition in accordance with ISO 10349-4. Use a test Portion of about 5,0 g and ignite in a platinum crucible (600 “6 t 50 OC, 4 h, 0,000 1 g)3)0 Wetain this residue for the heavy metals and iron content tests in 7.4 and 7.5. 3) The not
11、ation System used for the drying process procedure is given in ISO 10349-1. ISO 3299: 1994(E) I - 0 ISO 7.4 Heavy metals content 7.4.1 Specification Maximum content of heavy metals shall be 0,002 % (m/m). 7.42 Procedure NOTE 2 The Standard for the iron test (7.5) is prepared in the same way as the h
12、eavy metals Standard. Determine the percentage of heavy metals in accord- ante with ISO 103495. Use a test Portion of the residue from the ignition test (7.32) corresponding to 2 g of the Sample prepared in accordance with ISO 10349-5:1992, 7.1 (i.e. IO ml of the 25 ml residue Solution). Use 4 ml of
13、 heavy metals Standard prepared in accordance with ISO 10349-51992, 8.1.1. 75 . Iron content 7.5.1 Specification Maximum content of iron shall be 0,005 % (L T is the mass, in grams, of the crucible and residue; m2 is the mass, in grams, of the crucible; 100 is the factor for percentage. 4) Concern o
14、ver the use of halogenated hydrocarbons as solvents has resulted in a request for alternatives to the use of chloroform in this Pest procedure. Other solvents have not yet been evaluated and there is no information available on the applicability of other solvents in this test procedure. This is why this part of the specification is optional. 0 ISO Wave number, cm- ISO 3299: 1994( El Wavelength, pm Figure 1 - Reference infrared spectrum of l-phenyl-3-pyrazolidinone (KBr plate) 5
