Original standard number ZB G85005-90 HG/T 3574-1990 Photographic grade 4-hydroxy-6-methyl-1,3,3a,7-tetraazaindene (ST-1) HG/T3574-1990 Standard download decompression password: www.bzxz.net

Industry Standard of the People's Republic of China
ZB G85005:90
Adjusted to: Gh3r74-IPPo
4-Hydroxy-6-methyl-1,3,3a,7-tetrazolyl (ST-1)Published on 1990-04-17
Published by the Ministry of Chemical Industry of the People's Republic of China and implemented on 1990-10-01
Industry Standard of the People's Republic of China
Photographic Grade
4-Hydroxy-6-methyl-1,3,3.7-tetrazolyl (ST-1) This product is white powder.
Structural formula:
Molecular formula: CN1O
Relative molecular mass: 150.14 (according to the international atomic weight of 1987) 1 Main content and scope of application
ZB G85005-90
HGh3574-990
This standard specifies the technical requirements, test methods, inspection rules and packaging, marking, transportation and storage of photographic grade ST-1. This standard applies to ST-12 used in the preparation of photographic emulsions of light-sensitive materials. Reference standards
GB 602
GB 603
GB 617
GB 619
Chemical reagents Preparation of standard solutions for titration analysis (volume analysis) Preparation of standard solutions for determination of impurities of chemical reagents Preparation methods for preparations and products used in chemical reagent test methods General method for determination of melting point range of chemical reagents Sampling and acceptance rules for chemical reagents
GB 6682
GB9721
Laboratory water specifications
General rules for molecular absorption spectrophotometry of chemical reagents (ultraviolet and visible light parts)GB9723
General rules for flame atomic absorption spectrometry of chemical reagents 3 Technical requirements
3. 1 ST-1 (CHgN,0) content: 98. 5~101%. 3.2 Melting point range: 282~285℃.
3.3 Ultraviolet absorption spectrum, consistent with the ultraviolet absorption spectrum attached to this standard. 3.4 Photographic performance: qualified.
3.5 Solubility: qualified.
3.6 Maximum impurity content (measured in white content): Approved by the Ministry of Chemical Industry of the People's Republic of China on April 17, 1990 and implemented on October 1, 1990
Test method
Volatile matter
Iron (Fe)
Lead (Ph)
Copper (Ca)
Nickel (Ni)
Zinc (Zn)
Chromium (Cr)
4.1 Determination of ST-1 (CHN,O) content
ZB G85 005—
Weigh 0.3 g of sample, accurate to 0.0001 g, place in a 250 mL conical flask, add 50 mL of freshly boiled water, heat to dissolve, cool to room temperature, add 5 drops of phenol indicator solution (10 g/L.), and titrate with sodium hydride standard solution [c(NaOH)= to light pink.
The content (r1) of ST-1(C,HN,O) is calculated according to formula (1): ec
Wherein:
c(W,-Vo)x0.150
The percentage content of ST-1(C,HN,O), %;
The molar concentration of standard sodium hydroxide titration solution, mol/l.-When titrating the sample, the amount of standard sodium hydroxide titration solution used, mL; when titrating the blank, the amount of standard sodium hydroxide titration solution used, mL.t-The mass of the sample B;
=0. 1mol/L] Titrate until the solution changes from colorless to
0.1501--—The mass of ST-1 expressed in grams equivalent to 1. 00mL standard sodium hydroxide titration solution Cc(NaOJI)=1.000mol/L;
Parallel determination allows a deviation within 0.4%. 4.2 Determination of melting point range
Determine in accordance with the provisions of GB 619. 4.3 Determination of UV absorption spectrum
Weigh 1.5 mg of sample, place in a 150 mL beaker, add 120 mL of methanol and 10 mL of water, and shake to dissolve the sample. According to the provisions of GB9721, use a quartz absorption cell to measure its UV absorption spectrum in the wavelength range of 190~~350 nm. Use a blank solution as a reference solution. The standard UV absorption spectrum is shown in the figure below.
4.4 Determination of photographic performance
ZB G85 005—90
Drum's m)
ST-1 standard ultraviolet absorption spectrum
4.4.1 Standard sample
The supply and demand parties shall negotiate and take the medium and high samples with qualified physical and chemical test data as the standard sample. It shall be well stored and valid for two years. 4.4.2 Determination method
Each user shall use the current production formula, processing formula and process to test and compare the test samples and standard sample pieces after reverse artificial aging. The photographic performance is as follows:
8. The increase of gray fog is not more than 0.02;
b. The sensitivity decrease is not more than 10%.
4.5 Determination of solubility
ZB G85 005—90
Weigh 1.0g sample, accurate to 0.01g, place in a 250mL conical flask, add 100mL water, drop sodium hydroxide solution (40g/L) to make the solution pH reach 6.5~7.0, oscillate to dissolve, there should be no insoluble matter in the solution. 4.6 Determination of impurity content
4.6.1 Volatile matter
Weigh 1g sample in a weighing bottle with constant weight, accurate to 0.1mg, and dry at 105~110℃ to constant weight (about 3h). Volatile matter (X2) is calculated according to formula (2):
In the formula, X2-
Volatile matter percentage, %;
m—tg
Research 2: · Before drying, weigh the mass of the sample in the weighing bottle, : m
After drying, weigh the mass of the sample in the weighing bottle, ; The mass of the weighing bottle, .
Parallel determination allows a deviation within 0.05%. 4.6-2 Ash content
Weigh 3g of sample, weigh to 0.01g, place it in a porcelain crucible with constant weight, heat it on an electric furnace, and fully carbonize it. Then move it into a muffle furnace and burn it at 500±50℃ to constant weight (about 6h). The ash content (X) is calculated according to formula (3):
In the formula, X----% ash content, %, mi -
mass of added ash, g;
mass of exhaust gas, g;
mass of sample,.
Parallel determination allows a deviation within 0.05%, and the ash is retained for the determination of metal ion content. 4.6.3 Iron
Determine in accordance with the provisions of GB9723, where: 4.6.3.7 Instrument conditions
Light source: iron hollow cathode lamp
Wavelength: 248.3nm
Flame: air-acetylene
4.6.3.2 Determination method
Prepare 0.8, 1.6, 3.26.4, 12.8ppm iron (Fe) standard solutions respectively, and draw the working curve of iron. Add 2mL of hydrochloric acid to the crucible containing the retained ash in 4.6.2 to dissolve it, and transfer it to a 25.0mL volumetric flask. Add 1mL of nitric acid to the crucible to dissolve the residue, rinse the lid and cover with deionized water several times, transfer the solution to the above 25.0mL volumetric flask, and then dilute to the scale with deionized water, shake well, and measure according to the provisions of 6.2.1 of GB 9723. Perform a blank test under the same conditions.
The allowable deviation of parallel determination is within 1.0ppm. 4.6.4 Lead
Determine in accordance with the provisions of GB 9723, where: 4.6.4.1 Instrument conditions
Light source: lead hollow cathode lamp
Wavelength: 283.3nm
Flame: air-acetylene
4.6.4.2 Determination method
ZB G85005-90
Prepare 0.2, 0.4, 0.8, 1.6, 3.2 ppm lead (Pb) standard solutions respectively, and draw the T curve of lead. The following is the same as the determination method of 4.6.3.2 iron. The allowable deviation of parallel determination is within D.5ppm. 4.6.5 Copper
Determine in accordance with the provisions of GB9723, including: 4.6.5.1 Instrument conditions
Light source: copper hollow cathode lamp
Wavelength 324.7nm
Flame: air-acetylene
4.6.5.2 Determination method
Prepare 0.4, 0.8, 1.6, 3.2, 6.4ppm (Cu) standard solutions respectively, and draw the working line of copper. The following is the same as the determination method of iron.
The allowable deviation of parallel determination is within 0.5ppm. 4.6.6 Nickel
Determine in accordance with the provisions of GB9723, including
4.6.6.1 Instrument conditions
Light source: nickel hollow cathode lamp
Wavelength, 232.0nm
Flame: air-acetylene
4.6. 6.2 Determination method
Same as the determination method for sodium.
Parallel determination allows a deviation within 0.5ppm. 4.6.7 Zinc
Determine in accordance with the provisions of GB9723, where: Instrument conditions
4. 6-7. 1
Light source: zinc hollow cathode lamp
Wavelength: 213.8nm
Flame: air-acetylene
4. 6.7. 2 Determination method
Same as the determination method for iron.
Parallel determination allows a deviation within 1. Dppm. 4.6.8 Chromium
Determine in accordance with the provisions of GB9723. In particular:
4.6.8.1 Instrument conditionsbzxz.net
Light source: chromium hollow cathode lamp
Wavelength: 357.9nm
Flame: air-acetylene
4.6.8.2 Determination method
Same as the determination method for lead.
Parallel determination allows a deviation within 0.5ppm. 5 Inspection rules
Sampling and acceptance shall be carried out in accordance with the provisions of GB619. 6 Packaging, marking, transportation and purchase and storage
ZB G85 005—90
6.1 Packaging
Used iron barrels or other materials for outer packaging, inner plastic packaging and sealing. Packaging unit 5kB6.2 Marking
The barrel is enclosed with a product certificate. The outside of the barrel is labeled with the product name, label number, registered trademark, net weight, gross weight, production batch number, ex-factory date, manufacturer name and address. 6.3 Transportation and storage
Use various means of transportation. Do not invert or store with oxidants. Store in a dry, dark and cool place. Additional instructions:
This standard is proposed by the National Photographic Material Standardization Technical Committee. This standard is drafted by the Photographic Material Technology Development Center of the Ministry of Chemical Industry. The main drafters of this standard are Zhang Lian and Xun Xi Zeng. Copyright is reserved and may not be printed
Book number: 155066·2-7802
Price:
Standard month 155—68
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