Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T 2632—94
Photographic Grade Chemicals
General Test Methods
Published on 1994-08-17
Ministry of Chemical Industry of the People's Republic of China
Implemented on 1995-01-01
Chemical Industry Standard of the People's Republic of China
General Test Methods for Photographic Grade Chemicals
HG/T 2632 -- 94
Chapter 4 of this standard is equivalent to IS010349.2:1992 "Test methods for photographic grade chemicals Part 2 Determination of water-insoluble matter"; Chapter 6 is equivalent to IS010349.4:1992 "Test methods for photographic grade chemicals Part 4 Determination of ignition residue"; Chapter 7 is equivalent to IS010349.5:1992 "Test methods for photographic grade chemicals Part 5 Determination of heavy metals and iron"; Chapter 9 is equivalent to TS010349.7:1992 "Test methods for photographic grade chemicals Part 7 Determination of acidity or alkalinity" ： Chapter 10 is equivalent to ISO10349.8:1992 "Test methods for photographic grade chemicals Part 8 Determination of volatile substances", Chapter 11 is equivalent to ISO10349.9:1992 "Test methods for photographic grade chemicals Part 9 Determination of reaction with silver hydrogen nitrate solution", Chapter 12 is equivalent to ISO10349.10:1992 "Test methods for photographic grade chemicals Part 10 Determination of sulfide", Chapter 13 is equivalent to ISO10349.12:1992 "Test methods for photographic grade chemicals Part 12 Determination of density".
1 Subject content and scope of application
This standard specifies the general test methods for photographic grade chemicals, and this standard is applicable to photographic grade chemicals. 2 Reference standards
GB/T601 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T602 Preparation of standard solutions for determination of impurities of chemical reagents GB/T603 Preparation of preparations and products used in test methods of chemical reagents GB/T619 Sampling and acceptance rules for chemical reagents GB/T682 Specifications and test methods for water used in analytical laboratories 3 General rules
3.1 General provisions
Although the ultimate standard for testing photographic grade chemicals should be whether they can achieve better application results in appropriate application tests, the shorter and more economical test methods specified in this standard are usually appropriate. This standard does not specify many quantities involved in the test methods. These quantities are different for different photographic grade chemicals. These quantities should be specified in the product standards. The test methods specified in this standard involve many hazardous chemicals. When using them, refer to the relevant financial or user manual.
Old instrument tests can replace the test methods specified in this standard. However, when using instruments for testing, the precision of the instrument should meet the requirements of this standard or higher. The user may make appropriate adjustments to the test methods specified in this standard. 3.2 Definitions
This standard adopts the following definitions:
Approved by the Ministry of Chemical Industry of the People's Republic of China on August 17, 1994 and implemented on January 1, 1995
3.2.1 Photographic grade chemicals
HG/T 2632-94
Chemicals that meet certain quality standards and are used to process and process photosensitive materials that have been exposed. Such chemicals should not damage the inherent properties of photosensitive materials.
3.2.2 Density
In this standard, the density of a substance refers to the mass of a substance per unit volume at 25°C, expressed in g/mL. 3.3 Glassware
All heated glassware should be made of heat-resistant borosilicate glass. All measuring cylinders, measuring cups, volumetric flasks, pipettes, burettes and other volumetric instruments shall meet the requirements of Class A volumetric instruments. 34 Sampling
Sampling shall comply with the provisions of GB/T 619
4 Determination of water-insoluble matter
4.1 This method is not applicable to photographic grade chemicals that are unstable in boiling water or corrode glass filters. 4.2 Reagents
The water used in the experiment shall comply with the specifications of Grade III water in GB/T 6682 4.3 Instruments and devices
4.3.1 General laboratory instruments.
4.3.2 Glass filter: pore size is 10~15μm, 4.3.3 Vacuum suction filter device
4.3.4 Electric oven: temperature can be maintained at 105~115℃.4.3.5 Balance: sensitivity is 0.1mg.
4.4 Operation steps
Weigh the specified amount of sample, add it to a 125mL conical flask containing 100mL water, heat it on a steam bath for 30in, filter it with a glass filter crucible that has been dried at 105℃ for 1h and weighed (accurate to 1mg), wash the glass filter containing the filter residue with hot water, dry it at 105℃ for 4h, and weigh it (accurate to 1mg)4.5 Expression of results
The water-insoluble content x expressed as mass percentage is calculated according to formula (1),
where: ——
--mass of filter residue plus glass filter crucible, g;
m--mass of glass filter residue, g
mmass of sample, g.
5 Determination of ammonia insoluble matter
× 100
5.1 The ammonia insoluble matter in this method is the precipitate formed by calcium, magnesium and ammonia. 5.2 Reagents
5. 2.1 Ammonium oxalate ((NH4C,O, ·H4O) solution: 40 g/L: dissolve 40 g of ammonium oxalate in 500 mL of water and dilute to 1000 mL. 5.2.2 Diammonium hydrogen phosphate [(NH4HPO4) solution: 100 g/L: dissolve 10 g of diammonium hydrogen phosphate in 50 L of water and dilute to 500 L. 5.2.3 Ammonia nitrogen water (NH4OH) Solution: 1+9; Slowly add 10mL of ammonia water with a density of about 0.91 to 90mL of water and mix well. 2
5.2.4 Hydrogen water (NH,0H) solution: 1+39;HG / T 2632 --- 94
Slowly add 25mL of ammonia water with a density of about 0.91 to 975mL of water and mix well. 5.2.5 Experimental water: It should meet the specifications of grade 3 water in GB/T6682. 5.3 Instruments and devices
5.3.1 General laboratory instruments.
5.3.2: The capacity is 100mL or larger. According to the properties of the sample, choose ceramic, alumina, platinum or quartz glass.
5.3.3 High temperature furnace: can maintain 600℃ high temperature, accuracy is ±50T, 5.3.4 Balance: sensitivity is 0.1mg.
5.4 Operation steps
Weigh 10.0g sample (accurate to 0.1g), dissolve in 75mL water, add 5mL ammonium oxalate solution (40g/L), 4mL diammonium hydrogen phosphate solution (100g/L), 10mL ammonia solution (1+9), place for 8 h. If a precipitate is formed, filter it with ash-free filter paper of medium pore size (10μm～15μm), wash it with ammonia solution (1+39), transfer the filter paper and precipitate to a crucible that has been burned to constant weight at 600±50℃ (accurate to 1mg when weighing), carefully heat it on a blowtorch to ash, burn the residue in a high-temperature furnace at a specified temperature and within a specified time, cool it in a desiccator, and weigh it (accurate to 1mg). 5.5 Expression of results
The ignition residue expressed as a percentage of mass content is calculated according to formula (2): x,
where: m2 mass of residue added to crucible, g
ml--mass of crucible, g;
mass of sample,.
6 Determination of ignition residue
6.1 Instruments and devices
6.1.1 General laboratory instruments,
× 100
6.1.2 Crucible: capacity of 100mL or more. According to the properties of the sample, choose a crucible made of porcelain, alumina, platinum or quartz.
6.1.3 High temperature furnace: capable of maintaining a high temperature of 600℃, with an accuracy of ±50℃. 6.1.4 Balance: sensitivity of 0.1mg.
6.2 Operation steps
Weigh the specified sample (accurate to 0.01g), place it in a crucible that has been burned to constant weight at 600±50℃ (accurate to 1mg when weighing), heat it to carbonize, and drive out volatile substances. Then burn the crucible in a high temperature furnace at a specified temperature and within a specified time. Be careful not to lose ash. Cool it to room temperature in a desiccator and weigh it (accurate to 1mg). 6.3 Expression of results
The ignition residue expressed as mass percentage is calculated according to formula (3): x,
mz -m,
Where: m2-mass of the residue after burning, gim,\mass of the sample, g;
-mass of the sample, g.
× 100
7 Determination of gold and iron
7.1 Reagents
HG/T 2632 —94
The impurity standard solutions, preparations and products used in this determination method shall be prepared in accordance with the provisions of GB/T602 and GB/T603. The experimental water shall meet the specifications of grade 3 water in GB/T6682. 7.2 Instruments and devices
7.2.1 General laboratory instruments
7.2.2 Two matching 50mL Nessler colorimetric tubes. 7.3 Operating steps
7.3. 1 Prepare the sample
Depending on the nature of the sample, prepare the sample using one of the following methods. 7.3.1.1 Dissolve the ignition residue
Dissolve the ignition residue with 2 mL of hydrochloric acid solution (1+3) (see Chapter 6), rinse it with water into a 100 mL beaker, and add water to 25 mL.
7.3.1.2 Dissolve the sample with water
Weigh the specified amount of sample, add it to a 100 mL beaker, and dissolve it with 25 mL of water. 7.3.1.3 Dissolve the sample with water after treating it with acid Weigh the specified amount of sample, add it to a 100 mL beaker, and dissolve it with 25 mL of water. Slowly add 15 mL of hydrochloric acid with a density of about 1.18 g/mL, heat on a steam bath to evaporate to dryness, cool, and redissolve the residue with 25 mL of water. 7.3.2 Prepare the impurity standard solution
Depending on the nature of the sample. Prepare impurity standard solutions using one of the following methods: 7.3.2.1 Dilution with water
Pipette the specified amount of heavy metal standard solution and iron standard solution into two 100mL beakers and dilute each to 25mL with water
7.3.2.2 Treatment with acid
Pipette the specified amount of heavy metal standard solution and iron standard solution into two 100mL beakers and add 15mL of hydrochloric acid with a density of about 1.18B/mL to each beaker. Heat on a steam bath and evaporate to dryness. Redissolve each residue with 25mL of water. 7.3.3 Pretreatment of samples and impurities Treat the sample prepared in 7.3.1 and the two impurity standard solutions prepared in 7.3.2 as follows: add 2 drops of p-nitrophenol indicator (2.5 g/L) to each. If the solution is colorless, add aqueous ammonia solution (1+9) until the solution begins to turn yellow, then add hydrochloric acid solution (1+99) dropwise until the solution turns colorless, and then add 1 mL in excess. If the solution turns yellow after adding p-nitrophenol indicator (2.5 g/L), directly add hydrochloric acid solution (1+99) dropwise until the solution turns colorless, and then add 1 mL in excess. Dilute the sample and the two impurity standard solutions to 50 mL with water; mix well. 7.3.4 Test for heavy metals (expressed as Pb)
Add 5 mL of saturated hydrogen sulfide aqueous solution to 20 mL of treated sample and 20 mL of treated heavy metal standard solution, dilute with water to 50 mL, mix well, and transfer to two Nessler tubes. The color generated in the sample should not be darker than the color generated in the heavy metal standard bath solution.
7.3.5 Test for iron
Add 5 mL of 110-phenazone mixed solution to 20 mL of treated sample and 20 mL of treated iron standard solution. Instructions:
1J[SO10349.5 stipulates that 10 mL of sodium sulfide solution (50 g/L) should be added. Experiments show that since sodium sulfide solution has a strong alkalinity, the pH value of the sample increases after addition, and the indicator p-nitrobenzophenone turns yellow, making it impossible to test for heavy metals, so 5 mL of saturated hydrogen sulfide solution is added instead. 4
HG / T 2632 — 94
[Consists of equal volumes of 1,10-phenanthroline solution (1.0 g/L), hydroxylamine hydrochloride solution (100 g/L) and acetic acid-sodium acetate buffer solution with a pH value of 5], diluted with water to 50 mL, mixed evenly, and transferred to two Nessler colorimetric tubes. The color generated in the sample should not be darker than the color generated in the iron standard solution. Note: The determination of iron can also be replaced by spectrophotometry. 8 Determination of halides (expressed in)
8. 1 The detection range of this method is 0. 02～6μg/mL (in terms of CI) 8.2 Reagents
The impurity standard solutions, preparations and products used in this determination method shall be prepared in accordance with the provisions of GB/T602 and GB/T603. The experimental water shall meet the specifications of grade 3 water in GB/T6682 8, 3 Instruments and Apparatus
8.3.1 General Laboratory Instruments
8.3.2 Two matching 50mL Nessler colorimetric tubes. 8.4 Operating Procedure
Weigh 0.9~1.1g of sample and dissolve it in 200mL of water. Pipette 20mL of the above solution into a 50mL Nessler colorimetric tube, then add 5mL of nitric acid solution (1+9) and 1mL of silver nitrate solution (100g/L), dilute to 50mL, and mix. Compared with the standard comparison solution, the turbidity of the solution should not exceed that of the standard comparison solution. The preparation of the standard comparison solution is to pipette a specified amount of chloride standard solution and treat it in the same way as the sample. 9 Determination of Acidity and Alkalinity
9.1 Reagents
The standard titration solutions, preparations and products used in this determination method shall be prepared in accordance with the provisions of GB/T601 and GB/T603. The experimental water shall meet the specifications of Grade 3 water in GB/T6682. 9.2 Instruments and devices
General laboratory instruments.
9.3 Operation steps
Weigh the specified amount of sample, dissolve it in 100mL of carbon dioxide-free water, add 3-li phenol with indicator (1g/L), observe the color of the solution, if the solution is colorless, measure the acidity; if the solution turns pink, measure the alkalinity. 9.3.1 Determination of acidity
Use sodium hydroxide standard titration solution (0.01 mol/L) to titrate until the sample begins to turn pink and remains unchanged for 30 seconds. 9.3.2 Determination of alkalinity
Use hydrochloric acid standard titration solution (0.01 mal/L) to titrate until the sample begins to turn completely colorless. 9.4 Expression of results
9.4.1 Calculate the acidity x expressed as a percentage of mass according to formula (4),
where: c is the concentration of sodium hydroxide standard titration solution, mol/L; x 100
V——the amount of sodium hydroxide standard titration solution consumed when reaching the end point, mL; K-constant (0.1 multiplied by the molar mass of the acid being tested, g/m0lm—the mass of the sample, g.
0.4.2 Calculate the alkalinity x expressed as a percentage of mass according to formula (5) (4)
where: c
HG / T 2632 —94
-Concentration of hydrochloric acid standard titration solution, mol/L: X 100+Www.bzxZ.net
-The amount of hydrochloric acid standard titration solution consumed when reaching the end point, Ⅱ L; K——constant (0.1 multiplied by the mass of the base to be tested), g/ mol;m——mass of sample, g.
10 Determination of volatile substances
10.1 This method is applicable to phase-grade chemicals that can completely release volatile substances at 70-105°C. 10.2 Instruments and devices
10.2.1 General laboratory instruments.
10.2.2 Short stoppered weighing bottle: the container is 50L10.2.3 Electric oven: the temperature can be maintained at 70-105°C, and the temperature error is controlled to be ±5°C.10.2.4 Balance: the sensitivity is 0.1mg-
10.3 Operation steps
Weigh the specified amount The sample is placed in a short stoppered weighing bottle that has been dried at a specified temperature for 1 hour and weighed (accurate to 0.1 mg). The weighing bottle containing the sample is weighed (accurate to 0.1 mg). At the specified temperature, the weighing bottle is placed in an oven and dried to constant weight. 10.4 Expression of results
The volatile substance x expressed as a mass percentage is calculated according to formula (6)x
where: mz is the mass of the weighing bottle plus the sample before drying, g; m,--the mass of the weighing bottle after drying, g; mo--the mass of the weighing bottle, g.
11 Determination of reaction with ammoniacal silver nitrate solution
11.1 Reagents
× 100
The preparations and products used in this determination method shall be prepared in accordance with the provisions of GB/T603, and the experimental water shall meet the specifications of grade 3 water in GB/T6682. 11.2 Instruments and devices
11.2.1 General laboratory instruments.
11.2.2 Two matching 50mL Nessler colorimetric tubes, 11.3 Operation steps
Weigh 2.0g of sample (accurate to 0.1g), dissolve it in 40mL of water, transfer 20mL of the above solution into a Nessler colorimetric tube, and then add 10mL of newly prepared silver nitrate ammonia solution (density is about 0.91g/mL ammonia water and silver nitrate solution (100/L) are mixed in equal volumes), mixed evenly, left for 2 minutes, compared with the blank, the color or turbidity of the solution should not exceed that of the blank,
blank is At the same time, transfer the remaining 20mL of the above solution to another Nessler colorimetric tube, then add 5mL of nitrogen water with a density of about 0.91g/mL and 5mL of water, mix well, and leave for 2min. Note: After the test is completed, all test solutions and remaining preparations should be disposed of immediately, and the container should be cleaned to prevent the formation of explosive compounds (feather-like powder or silver azide) after standing. 6
12 Determination of sulfide
HG/T2632—94
12.1 The detection range of this method is 0.04~0.2/mL (in s). 12.2 Reagents
The impurity standard solutions, preparations and products used in this determination method are prepared in accordance with the provisions of GB/T602 and GB/T603. The experimental water should meet the specifications of grade 3 water in GB/T6682. 12.3 Instruments and devices
12.3.1 General laboratory instruments.
12.3.2 Two matching 50mL Nessler colorimetric tubes. 12. 4 Operation steps
Weigh 2.0g sample (accurate to 0.1g) and dissolve it in 25mL container. Transfer the above solution to a Nessler colorimetric tube, then add 2mL of lead hydroxide solution [add an appropriate amount of sodium hydroxide solution (100g/L) to the lead acetate solution (100g/L) to dissolve the newly formed precipitate, and add a slight excess), dilute to 50mL, mix well, and compare with the standard comparison solution. The dark color generated by the solution should not be darker than that of the standard comparison solution. The preparation of the standard comparison solution is to transfer a specified amount of sulfide standard solution and treat it in the same way as the sample. 13 Density determination
13.1 Reagents
The water used in the determination should meet the specifications of Grade III water in GB/T6682. 13.2 Instruments and devices
13. 2. 1 General laboratory instruments
13.2.2 Densitometer: The measurement accuracy is 0.001 unit. 13.2.3 Densitometer tube: A cylindrical glass container with a volume of about 250mL and higher than the densitometer. 13.2.4 Constant temperature water bath: There is a heating system that can maintain circulation and constant temperature (±0.05℃). The water bath should be deep enough to ensure that the sample in the densitometer tube is below the water surface. The water margin should be 25℃. 13.3 Operating steps
Add 100mL of sample to a dry and clean densitometer tube, place the densitometer tube in the water bath, and after the sample and water bath temperatures reach equilibrium, measure the density with the densitometer according to the instructions. Additional notes:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard was drafted by the Photosensitive Material Technology Development Center of the Ministry of Chemical Industry. This standard was funded by the Photosensitive Material Technology Development Center of the Ministry of Chemical Industry. The main drafters of this standard were Fang Liwen and Zhang Dade. People's Republic of China
Chemical Industry Standard
General Test Methods for Photographic Grade Chemicals
HG/T2632-94
Editor: Chemical Industry Standard Compilation and Publishing Group
(Standardization Institute of the Ministry of Chemical Industry)
Postal Code: 100011
Printed by Standardization Institute of the Ministry of Chemical Industry
Copyright reserved. No reproduction allowed
Format: 880×12301/16Printing Sheet Count: 14000First Printing in October 1997
Edition 1 in October 1997
Print Count: 1500
Book Fee: 5.00 Yuan
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