Some standard content:
ICS31-030
Registration No.: 7051997
Electronic Industry Standard of the People's Republic of China
SJ/T11136-1997
Zirconium dioxide used for electronic ceramics
ceramics1997-09-03 Issued
1998-01-01 Implementation
The Ministry of Electronics Industry of the People's Republic of China IssuedTYYKAONKAca
1 Scope
2 Reference standards
3 Classification and naming
5 Test methods
6 Inspection rules
7 Marking, packaging, transportation and storage
Appendix A (Standard Appendix)
Appendix B (Suggestive Appendix)
Determination of C1
Treatment of mercury-containing waste liquid
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This standard is formulated to meet the needs of the development of scientific research and production of electronic ceramics in my country and to facilitate the improvement and stability of the quality of zirconium dioxide.
The formulation of this standard is conducive to my country's products of this type to catch up with the international advanced level, enhance the competitiveness in the international market, and promote product exports.
Appendix A of this standard is the standard appendix;
Appendix B of this standard is the indicative appendix.
This standard is under the jurisdiction of the Standardization Institute of the Ministry of Electronics Industry. The drafting units of this standard are: Jiaozuo Chemical General Plant, Standardization Institute of the Ministry of Electronics Industry, and State-owned Factory No. 798. The main drafters of this standard are: Sun Yaguang, Xu Qing, Shang Jianyu, Wang Yugong, Qiu Yuexia, YKAoNrKAas
1 Scope
Electronic Industry Standard of the People's Republic of China
Zirconium dioxide used for
electronic ceramics
SJ/T11136-1997
This standard specifies the classification, requirements, test methods, inspection rules, marking, packaging, transportation, storage, etc. of zirconium dioxide used for electronic ceramics.
This standard applies to zirconium dioxide used for electronic ceramics (hereinafter referred to as zirconium dioxide). 2 Reference Standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards.
Determination of zirconium oxide and hafnium oxide in zirconium oxide and hafnium amide-Mandelic acid gravimetric method GB/T2590.1—1981
GB/T2590.2—1981
CB/T2590.3—1981
GB/T2590.4—1981
GR/T2590.5—1981
G/T2590.6—1981
GB/T5061—1985
GB/T6524—1986
GB/T13390—1992
3 Classification and nomenclature
Determination of iron in zirconium oxide and hafnium oxide-Sulfosalicylic acid Absorption photometry Determination of silicon content in zirconium oxide and hafnium oxide Silica molybdenum blue absorption photometry Determination of aluminium content in zirconium oxide and hafnium oxide Chrome azuro S-tetradecylpyridine fluoride absorption photometry
Determination of sodium content in zirconium oxide and hafnium oxide Flame atomic absorption spectrophotometry Diantipyrimethane absorption photometry
Determination of titanium content in zirconium oxide and hafnium oxide
Determination of bulk density of metal powders
Determination of particle size distribution of metal powders
Determination of specific surface area of metal powders
Part 3: Vibrating funnel method
Light transmission method
Nitrogen adsorption method
3.1 Classification
Zirconium dioxide can be divided into three categories and six models according to its performance and use requirements, as shown in Table 1. Table 1 Classification and model of zirconium dioxide
Irregular granular zirconium dioxide
Fine-grained zirconium dioxide
Ultrafine zirconium dioxide
Type approved by the Ministry of Electronics Industry of the People's Republic of China on September 3, 1997
EZ1-1, EZI-2
EZI-1, EZ2-2, EZ2-3
Implementation on January 1, 1998
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3.2 Naming
SJ/T11136-1997
The naming method of zirconium dioxide models is as follows. E
4 Requirements
4.1 Appearance
Indicates grade
Indicates category
Indicates zirconium dioxide
Indicates electronic use
Irregular granular zirconium dioxide is white and has a metallic luster. Fine-grained zirconium dioxide and ultrafine zirconium dioxide are both self-color powders.
4.2 Chemical composition and physical properties of zirconium dioxide The chemical composition and physical properties of zirconium dioxide are shown in Table 2. Table 2 Chemical and physical properties of ZrO2
Category model
ZrO2 + HfO2
Ignition loss mass
Average particle size (um)
Bulk density (g/cm2)
Specific surface area (m2/g)
Test method
5.1 Determination of chemical composition
rYKAOMrKAa
SJ/T11136—1997
5.1.11.2 Class 2 ZrO2 + HfO2 content shall be determined by the method specified in GB/T2590.1. 5.1.2 Class 3 ZrO + HfO2 content shall be determined by the method of 100 minus impurities. 5.1.3 The contents of Fe2O3, SiO2, TiO2, Na2O and Al2O shall be determined by the methods specified in GB/T2590.2~2590.6. 5.2 The determination method of C1 is shown in Appendix A (Standard Appendix). The treatment of waste liquid containing mercury is shown in Appendix B (Suggestive Appendix). 5.3 Determination of moisture content Weigh about 2g of the sample (accurate to 0.0002g) and place it in a weighing bottle that has been kept at a constant weight at 105℃~110℃, then dry it at 105℃~110℃ for 2h, cool it to room temperature in a dryer, and dry it repeatedly until it is kept at a constant weight. The mass percentage of moisture is calculated as follows: H0=\1=m2×100%. Where: H20—mass percentage of moisture Mass percentage: %; m1—mass of the sample before drying, g;
—mass of the sample after drying, g.
5.4 Determination of loss on ignition
Weigh about 1.5g of the sample (accurate to 0.0002g) and place it in a porcelain pot that has been burned to constant weight at 950℃. After weighing, place it in a muffle furnace with the lid half open and gradually heat it to 950℃, and keep it at this temperature for 45 minutes. After cooling to room temperature in a dryer, weigh it and repeatedly burn it at 950℃ to constant weight. The mass percentage of loss on ignition is calculated according to the following formula: Loss on ignition = 1 = m2×100%
Where: Loss on ignition—mass percentage of loss on ignition: %; mi
Mass of the sample before ignition, g:
—Mass of the sample after ignition. , g.
5.5 Determination of average particle size
The average particle size shall be determined in accordance with GB/T6524. 5.6 Determination of bulk density
The bulk density shall be determined in accordance with GB/T5061. 5.7 Determination of specific surface area
The specific surface area shall be determined in accordance with GB/T13390. 6 Inspection rules
6.1 Inspection classification
Product inspection is divided into acceptance inspection and routine inspection. 6.2 Sampling and batching rules
(2)
Take 500kg as a batch (less than 500kg can still be considered as a batch, but the total sampling weight shall not be less than 1kg), and randomly select 10% of the total number of pieces in the batch. When sampling, remove 100m of the surface. m material layer, use a clean and dry sampler or glass tube, insert it vertically from the center to 1/2 depth to take samples. Each batch of samples shall not be less than 1kg. Mix the sample thoroughly, reduce it to 500g by quartering method, and pack it into two clean and dry ground-mouth bottles, seal them, and label them with the manufacturer name, product name, model, batch number and sampling month. One bottle is used for inspection and the other is kept for future reference. 6.3 Delivery inspection
6.3.1 Delivery inspection must be carried out on zirconium dioxide when it is delivered. The inspection items are zirconium oxide, hafnium oxide content, iron oxide, silicon dioxide, sodium oxide content and loose density, average particle size and appearance. 6.3.2 If the indicators of all samples in the test meet the requirements of 4.1 and Table 2 of this standard, the batch of zirconium dioxide is considered qualified. If one or more items do not meet the requirements of 4.1 and Table 2 of this standard, double sampling should be done from the same batch, and the unqualified items should be re-inspected. If the re-inspection still fails, the batch of products is unqualified. 6.4 Routine inspection
6.4.1 Routine inspection is carried out on the qualified batch of delivery inspection, and at least once a year. When there are major changes in raw materials and production processes, routine inspection is also required. 6.4.2 Routine inspection items are shown in Table 2 and appearance is added. 6.4.3 If the indicators of all samples in the test meet the requirements of 4.1 and Table 2 of this standard, the zirconium dioxide is considered qualified. If one or more items do not meet the requirements of 4.1 and Table 2 of this standard, double sampling should be done, and the unqualified items should be re-inspected. If the re-inspection still fails, the routine inspection is unqualified. 6.5 When the supply and demand parties have disputes over product quality, they shall handle it in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
7 Marking, packaging, transportation and storage
7.1 Marking
A firm and clear mark shall be applied on the outer packaging, indicating the manufacturer's name, product name, model, net weight, manufacturing date, trademark and this standard number. The product certificate shall be attached to the inner packaging. Its contents include the manufacturer's name, product name, trademark, model, manufacturing date and this standard number.
7.2 Packaging
Zirconium dioxide is packaged in kraft paper barrels, iron barrels, three-in-one plastic woven bags, etc. Two layers of polyethylene plastic bags and one layer of plastic woven bags are used for inner packaging. Each piece shall not exceed 25kg. 7.3 Transportation
This product can be transported by any means. During transportation, pay attention to gentle unloading to prevent damage, rain and moisture. 7.4 Storage
This product should be stored in a ventilated and dry warehouse. 4
rYKAoNrKAcas
A1 Method Summary
SJ/T11136-1997
Appendix A
(Suggestive Appendix)
Determination of C1-
The sample is soaked in water and filtered. The filtrate is placed in slightly acidic water or ethanol aqueous solution. The chloride ions are converted into weakly ionized mercuric fluoride using a strongly ionized mercuric nitrate standard solution. Diphenylazocarbonyl hydrazide is used as an indicator to form a purple-red complex with excess Hg2+ to determine the end point.
A2 Reagents and Materials
A2.1 1+1 (V/V) and 1mol/L nitric acid solution (superior grade). A2.2 95% ethanol solution.
A2.3 Bromophenol blue indicator; 0.1% ethanol solution. A2.4 Diphenylazocarbonyl indicator; 0.5% ethanol solution, which should be re-prepared when the color change is not sensitive. A2.5 1mol/L sodium hydroxide solution.
A2.6 Sodium fluoride standard solution:
a) 0.05mol/L standard solution: weigh 2.9222g of standard sodium chloride that has been pre-burned at 500℃～600℃ for 1h and cooled in a desiccator, put it in a beaker, add a small amount of water to dissolve, transfer all the solution into a 1000ml volumetric flask, add water to the scale, and shake well.
b) 0.001mol/L or other concentration standard solution: accurately dilute the 0.05mol/L standard solution to the required multiple. A2.7 Mercuric nitrate standard solution:
a) 0.025mol/L standard solution: weigh 8.57g mercuric nitrate [Hg(Nox)2H,O], put it in a 250ml beaker, add 7ml 1+1 nitric acid solution, add a small amount of water to dissolve and filter, transfer to a 1000ml volumetric flask, add water to the scale and shake well; b) 0.005mol/L0.001mol/L or other concentration mercuric nitrate standard solution: accurately dilute the 0.025mol/L mercuric nitrate standard solution to the required multiple. When diluting, add an appropriate amount of 1:1 nitric acid solution to prevent the hydrolysis of mercuric nitrate: c) Calibration method of 0.025mol/L, 0.005mol/L, 0.001mol/L or other concentrations of mercuric nitrate standard solution: Accurately transfer 5.00ml of the corresponding sodium chloride standard solution, place it in a conical flask, add 5ml of water, 30ml of ethanol and 2 drops of bromophenol blue indicator, and add 1mol/L nitric acid solution until the solution changes from blue to yellow, then add 2~3 drops in excess, add 1ml of benzyl azocarbonyl indicator, and titrate with the corresponding concentration of mercuric nitrate standard solution until the solution changes from yellow to purple-red, which is the end point. At the same time, perform an empty mouth test. Keep the mercury-containing waste liquid after titration and treat it according to Appendix B. The concentration of nitric acid multiplied by the standard titration solution is calculated as follows: C,x Vi
C=2(VV,)
Wherein: C is the actual concentration of the standard titration solution of mercuric nitrate, mol/L; C is the concentration of the standard titration solution of sodium chloride, mol/L; V is the volume of the standard titration solution of mercuric nitrate consumed in the titration, ml; V is the volume of the standard titration solution of mercuric nitrate consumed in the blank titration, ml. A3 Analysis steps
YKAONrKAcas
（A1)
A3.1 Test material
SJ/T11136-1997
Weigh 10g of test material (all test material grinding rates are 100 days), accurate to 0.01g. A3.2 Determination
A3.2.1 Place the sample (A3.1) in a 250ml beaker, add 100ml water, cover with a watch glass, stir every 6min, immerse for 1h, filter with double-layer filter paper, collect the filtrate in a 100ml beaker, and when the filtrate is 15ml, rinse the beaker with the filtrate, pour out the filtrate, and then continue to collect the filtrate in this beaker until the filtration is completed. A3.2.2 Pipette 25.00ml of the test solution (A3.2.1) into a 300ml conical flask and add 75ml of ethanol. Add 4~5 drops of bromocresol blue indicator. If the solution is yellow, add 1mol/L sodium hydroxide solution until it turns blue, then add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess: If the solution is blue, add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess. Add 1ml of diphenylazocarbonyl indicator to the sample solution, and titrate with a standard solution of mercuric nitrate of appropriate concentration (the titration volume of the standard solution of mercuric nitrate is controlled at 7-15ml) until the solution changes from yellow to purple-red, which is the end point. At the same time, perform a blank test. A3.3 Expression of analysis results:
The mass percentage of chloride (in terms of CI) is calculated as follows: 2c(V-Vo)×35.45
m×100
Where: C1--mass percentage of CI\, %; 100%
C——actual concentration of standard solution of mercuric nitrate, mol/L.; V-volume of standard solution of mercuric nitrate consumed by the test solution, ml; Vo-volume of standard solution of mercuric nitrate consumed by the blank test, ml; V-volume of the test solution absorbed, ml;
m-mass of the sample, g.
YYKAONrKACas
·（A2）
SJ/T11136-1997
Appendix B
（Suggested Appendix）
Treatment of waste liquid containing mercury
In order to prevent the pollution of wastewater, it is recommended to treat the waste liquid obtained after the determination of chloride by mercury titration as follows. Collect the waste liquid after the determination in a container of appropriate size (such as: 50L), precipitate mercury with excess sodium sulfide in alkaline medium, and oxidize excess sodium sulfide with hydrogen peroxide to prevent mercury from dissolving in the form of polysulfide. Operation procedure: Collect the waste liquid in a container of about 50L. When the waste liquid reaches about 40L, add 400ml 40% sodium hydroxide solution and 100g sodium sulfide nonahydrate in sequence. After 10 minutes, slowly add 400ml 30% hydrogen peroxide solution and mix thoroughly. After 24 hours, drain the upper clear liquid into the waste water and transfer the sediment to another container for mercury recovery by a dedicated person.5 When the supply and demand parties have disputes over product quality, they shall handle it in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
7 Marking, packaging, transportation and storage
7.1 Marking
A firm and clear mark shall be applied on the outer packaging, indicating the manufacturer's name, product name, model, net weight, manufacturing date, trademark and this standard number. The product certificate shall be attached to the inner packaging. Its contents include the manufacturer's name, product name, trademark, model, manufacturing date and this standard number.
7.2 Packaging
Zirconium dioxide is packaged in kraft paper barrels, iron barrels, three-in-one plastic woven bags, etc. Two layers of polyethylene plastic bags and one layer of plastic woven bags are used for inner packaging. Each piece shall not exceed 25kg. 7.3 Transportation
This product can be transported by any means. During transportation, pay attention to gentle unloading to prevent damage, rain and moisture. 7.4 Storage
This product should be stored in a ventilated and dry warehouse. 4
rYKAoNrKAcas
A1 Method Summary
SJ/T11136-1997
Appendix A
(Suggestive Appendix)
Determination of C1-
The sample is soaked in water and filtered. The filtrate is placed in slightly acidic water or ethanol aqueous solution. The chloride ions are converted into weakly ionized mercuric fluoride using a strongly ionized mercuric nitrate standard solution. Diphenylazocarbonyl hydrazide is used as an indicator to form a purple-red complex with excess Hg2+ to determine the end point.
A2 Reagents and Materials
A2.1 1+1 (V/V) and 1mol/L nitric acid solution (superior grade). A2.2 95% ethanol solution.
A2.3 Bromophenol blue indicator; 0.1% ethanol solution. A2.4 Diphenylazocarbonyl indicator; 0.5% ethanol solution, which should be re-prepared when the color change is not sensitive. A2.5 1mol/L sodium hydroxide solution.
A2.6 Sodium fluoride standard solution:
a) 0.05mol/L standard solution: weigh 2.9222g of standard sodium chloride that has been pre-burned at 500℃～600℃ for 1h and cooled in a desiccator, put it in a beaker, add a small amount of water to dissolve, transfer all the solution into a 1000ml volumetric flask, add water to the scale, and shake well.
b) 0.001mol/L or other concentration standard solution: accurately dilute the 0.05mol/L standard solution to the required multiple. A2.7 Mercuric nitrate standard solution:
a) 0.025mol/L standard solution: weigh 8.57g mercuric nitrate [Hg(Nox)2H,O], put it in a 250ml beaker, add 7ml 1+1 nitric acid solution, add a small amount of water to dissolve and filter, transfer to a 1000ml volumetric flask, add water to the scale and shake well; b) 0.005mol/L0.001mol/L or other concentration mercuric nitrate standard solution: accurately dilute the 0.025mol/L mercuric nitrate standard solution to the required multiple. When diluting, add an appropriate amount of 1:1 nitric acid solution to prevent the hydrolysis of mercuric nitrate: c) Calibration method of 0.025mol/L, 0.005mol/L, 0.001mol/L or other concentrations of mercuric nitrate standard solution: Accurately transfer 5.00ml of the corresponding sodium chloride standard solution, place it in a conical flask, add 5ml of water, 30ml of ethanol and 2 drops of bromophenol blue indicator, and add 1mol/L nitric acid solution until the solution changes from blue to yellow, then add 2~3 drops in excess, add 1ml of benzyl azocarbonyl indicator, and titrate with the corresponding concentration of mercuric nitrate standard solution until the solution changes from yellow to purple-red, which is the end point. At the same time, perform an empty mouth test. Keep the mercury-containing waste liquid after titration and treat it according to Appendix B. The concentration of nitric acid multiplied by the standard titration solution is calculated as follows: C,x Vi
C=2(VV,)
Wherein: C is the actual concentration of the standard titration solution of mercuric nitrate, mol/L; C is the concentration of the standard titration solution of sodium chloride, mol/L; V is the volume of the standard titration solution of mercuric nitrate consumed in the titration, ml; V is the volume of the standard titration solution of mercuric nitrate consumed in the blank titration, ml. A3 Analysis steps
YKAONrKAcas
（A1)
A3.1 Test material
SJ/T11136-1997
Weigh 10g of test material (all test material grinding rates are 100 days), accurate to 0.01g. A3.2 Determination
A3.2.1 Place the sample (A3.1) in a 250ml beaker, add 100ml water, cover with a watch glass, stir every 6min, immerse for 1h, filter with double-layer filter paper, collect the filtrate in a 100ml beaker, and when the filtrate is 15ml, rinse the beaker with the filtrate, pour out the filtrate, and then continue to collect the filtrate in this beaker until the filtration is completed. A3.2.2 Pipette 25.00ml of the test solution (A3.2.1) into a 300ml conical flask and add 75ml of ethanol. Add 4~5 drops of bromocresol blue indicator. If the solution is yellow, add 1mol/L sodium hydroxide solution until it turns blue, then add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess: If the solution is blue, add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess. Add 1ml of diphenylazocarbonyl indicator to the sample solution, and titrate with a standard solution of mercuric nitrate of appropriate concentration (the titration volume of the standard solution of mercuric nitrate is controlled at 7-15ml) until the solution changes from yellow to purple-red, which is the end point. At the same time, perform a blank test. A3.3 Expression of analysis results:
The mass percentage of chloride (in terms of CI) is calculated as follows: 2c(V-Vo)×35.45
m×100
Where: C1--mass percentage of CI\, %; 100%
C——actual concentration of standard solution of mercuric nitrate, mol/L.; V-volume of standard solution of mercuric nitrate consumed by the test solution, ml; Vo-volume of standard solution of mercuric nitrate consumed by the blank test, ml; V-volume of the test solution absorbed, ml;
m-mass of the sample, g.
YYKAONrKACas
·（A2）
SJ/T11136-1997
Appendix B
（Suggested Appendix）
Treatment of waste liquid containing mercury
In order to prevent the pollution of wastewater, it is recommended to treat the waste liquid obtained after the determination of chloride by mercury titration as follows. Collect the waste liquid after the determination in a container of appropriate size (such as: 50L), precipitate mercury with excess sodium sulfide in alkaline medium, and oxidize excess sodium sulfide with hydrogen peroxide to prevent mercury from dissolving in the form of polysulfide. Operation procedure: Collect the waste liquid in a container of about 50L. When the waste liquid reaches about 40L, add 400ml 40% sodium hydroxide solution and 100g sodium sulfide nonahydrate in sequence. After 10 minutes, slowly add 400ml 30% hydrogen peroxide solution and mix thoroughly. After 24 hours, drain the upper clear liquid into the waste water and transfer the sediment to another container for mercury recovery by a dedicated person.5 When the supply and demand parties have disputes over product quality, they shall handle it in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection".
7 Marking, packaging, transportation and storage
7.1 Marking
A firm and clear mark shall be applied on the outer packaging, indicating the manufacturer's name, product name, model, net weight, manufacturing date, trademark and this standard number. The product certificate shall be attached to the inner packaging. Its contents include the manufacturer's name, product name, trademark, model, manufacturing date and this standard number.
7.2 Packaging
Zirconium dioxide is packaged in kraft paper barrels, iron barrels, three-in-one plastic woven bags, etc. Two layers of polyethylene plastic bags and one layer of plastic woven bags are used for inner packaging. Each piece shall not exceed 25kg. 7.3 Transportation
This product can be transported by any means. During transportation, pay attention to gentle unloading to prevent damage, rain and moisture. 7.4 Storage
This product should be stored in a ventilated and dry warehouse. 4
rYKAoNrKAcas
A1 Method Summary
SJ/T11136-1997
Appendix A
(Suggestive Appendix)
Determination of C1-
The sample is soaked in water and filtered. The filtrate is placed in slightly acidic water or ethanol aqueous solution. The chloride ions are converted into weakly ionized mercuric fluoride using a strongly ionized mercuric nitrate standard solution. Diphenylazocarbonyl hydrazide is used as an indicator to form a purple-red complex with excess Hg2+ to determine the end point.
A2 Reagents and Materials
A2.1 1+1 (V/V) and 1mol/L nitric acid solution (superior grade). A2.2 95% ethanol solution.
A2.3 Bromophenol blue indicator; 0.1% ethanol solution. A2.4 Diphenylazocarbonyl indicator; 0.5% ethanol solution, which should be re-prepared when the color change is not sensitive. A2.5 1mol/L sodium hydroxide solution.
A2.6 Sodium fluoride standard solution:
a) 0.05mol/L standard solution: weigh 2.9222g of standard sodium chloride that has been pre-burned at 500℃～600℃ for 1h and cooled in a desiccator, put it in a beaker, add a small amount of water to dissolve, transfer all the solution into a 1000ml volumetric flask, add water to the scale, and shake well.
b) 0.001mol/L or other concentration standard solution: accurately dilute the 0.05mol/L standard solution to the required multiple. A2.7 Mercuric nitrate standard solution:
a) 0.025mol/L standard solution: weigh 8.57g mercuric nitrate [Hg(Nox)2H,O], put it in a 250ml beaker, add 7ml 1+1 nitric acid solution, add a small amount of water to dissolve and filter, transfer to a 1000ml volumetric flask, add water to the scale and shake well; b) 0.005mol/L0.001mol/L or other concentration mercuric nitrate standard solution: accurately dilute the 0.025mol/L mercuric nitrate standard solution to the required multiple. When diluting, add an appropriate amount of 1:1 nitric acid solution to prevent the hydrolysis of mercuric nitrate: c) Calibration method of 0.025mol/L, 0.005mol/L, 0.001mol/L or other concentrations of mercuric nitrate standard solution: Accurately transfer 5.00ml of the corresponding sodium chloride standard solution, place it in a conical flask, add 5ml of water, 30ml of ethanol and 2 drops of bromophenol blue indicator, and add 1mol/L nitric acid solution until the solution changes from blue to yellow, then add 2~3 drops in excess, add 1ml of benzyl azocarbonyl indicator, and titrate with the corresponding concentration of mercuric nitrate standard solution until the solution changes from yellow to purple-red, which is the end point. At the same time, perform an empty mouth test. Keep the mercury-containing waste liquid after titration and treat it according to Appendix B. The concentration of nitric acid multiplied by the standard titration solution is calculated as follows: C,x Vi
C=2(VV,)
Wherein: C is the actual concentration of the standard titration solution of mercuric nitrate, mol/L; C is the concentration of the standard titration solution of sodium chloride, mol/L; V is the volume of the standard titration solution of mercuric nitrate consumed in the titration, ml; V is the volume of the standard titration solution of mercuric nitrate consumed in the blank titration, ml. A3 Analysis steps
YKAONrKAcas
（A1)
A3.1 Test material
SJ/T11136-1997
Weigh 10g of test material (all test material grinding rates are 100 days), accurate to 0.01g. A3.2 Determination
A3.2.1 Place the sample (A3.1) in a 250ml beaker, add 100ml water, cover with a watch glass, stir every 6min, immerse for 1h, filter with double-layer filter paper, collect the filtrate in a 100ml beaker, and when the filtrate is 15ml, rinse the beaker with the filtrate, pour out the filtrate, and then continue to collect the filtrate in this beaker until the filtration is completed. A3.2.2 Pipette 25.00ml of the test solution (A3.2.1) into a 300ml conical flask and add 75ml of ethanol. Add 4~5 drops of bromocresol blue indicator. If the solution is yellow, add 1mol/L sodium hydroxide solution until it turns blue, then add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess: If the solution is blue, add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess. Add 1ml of diphenylazocarbonyl indicator to the sample solution, and titrate with a standard solution of mercuric nitrate of appropriate concentration (the titration volume of the standard solution of mercuric nitrate is controlled at 7-15ml) until the solution changes from yellow to purple-red, which is the end point. At the same time, perform a blank test. A3.3 Expression of analysis results:
The mass percentage of chloride (in terms of CI) is calculated as follows: 2c(V-Vo)×35.45
m×100
Where: C1--mass percentage of CI\, %; 100%
C——actual concentration of standard solution of mercuric nitrate, mol/L.; V-volume of standard solution of mercuric nitrate consumed by the test solution, ml; Vo-volume of standard solution of mercuric nitrate consumed by the blank test, ml; V-volume of the test solution absorbed, ml;
m-mass of the sample, g.
YYKAONrKACas
·（A2）
SJ/T11136-1997
Appendix B
（Suggested Appendix）
Treatment of waste liquid containing mercury
In order to prevent the pollution of wastewater, it is recommended to treat the waste liquid obtained after the determination of chloride by mercury titration as follows. Collect the waste liquid after the determination in a container of appropriate size (such as: 50L), precipitate mercury with excess sodium sulfide in alkaline medium, and oxidize excess sodium sulfide with hydrogen peroxide to prevent mercury from dissolving in the form of polysulfide. Operation procedure: Collect the waste liquid in a container of about 50L. When the waste liquid reaches about 40L, add 400ml 40% sodium hydroxide solution and 100g sodium sulfide nonahydrate in sequence. After 10 minutes, slowly add 400ml 30% hydrogen peroxide solution and mix thoroughly. After 24 hours, drain the upper clear liquid into the waste water and transfer the sediment to another container for mercury recovery by a dedicated person.0.5mol/L standard solution: weigh 2.9222g of standard sodium chloride that has been pre-calcined at 500℃～600℃ for 1h and cooled in a desiccator, place it in a beaker, add a small amount of water to dissolve, transfer all the solution into a 1000ml volumetric flask, add water to the scale, and shake well.
b) 0.001mol/L or other concentration standard solution: accurately dilute the 0.05mol/L standard solution to the required multiple. A2.7 Mercuric nitrate standard solution:
a) 0.025mol/L standard solution: weigh 8.57g mercuric nitrate [Hg(Nox)2H,O], put it in a 250ml beaker, add 7ml 1+1 nitric acid solution, add a small amount of water to dissolve and filter, transfer to a 1000ml volumetric flask, add water to the scale and shake well; b) 0.005mol/L0.001mol/L or other concentration mercuric nitrate standard solution: accurately dilute the 0.025mol/L mercuric nitrate standard solution to the required multiple. When diluting, add an appropriate amount of 1:1 nitric acid solution to prevent the hydrolysis of mercuric nitrate: c) Calibration method of 0.025mol/L, 0.005mol/L, 0.001mol/L or other concentrations of mercuric nitrate standard solution: Accurately transfer 5.00ml of the corresponding sodium chloride standard solution, place it in a conical flask, add 5ml of water, 30ml of ethanol and 2 drops of bromophenol blue indicator, and add 1mol/L nitric acid solution until the solution changes from blue to yellow, then add 2~3 drops in excess, add 1ml of benzyl azocarbonyl indicator, and titrate with the corresponding concentration of mercuric nitrate standard solution until the solution changes from yellow to purple-red, which is the end point. At the same time, perform an empty mouth test. Keep the mercury-containing waste liquid after titration and treat it according to Appendix B. The concentration of nitric acid multiplied by the standard titration solution is calculated as follows: C,x Vi
C=2(VV,)
Wherein: C is the actual concentration of the standard titration solution of mercuric nitrate, mol/L; C is the concentration of the standard titration solution of sodium chloride, mol/L; V is the volume of the standard titration solution of mercuric nitrate consumed in the titration, ml; V is the volume of the standard titration solution of mercuric nitrate consumed in the blank titration, ml. A3 Analysis steps
YKAONrKAcas
（A1)
A3.1 Test material
SJ/T11136-1997
Weigh 10g of test material (all test material grinding rates are 100 days), accurate to 0.01g. A3.2 Determination
A3.2.1 Place the sample (A3.1) in a 250ml beaker, add 100ml water, cover with a watch glass, stir every 6min, immerse for 1h, filter with double-layer filter paper, collect the filtrate in a 100ml beaker, and when the filtrate is 15ml, rinse the beaker with the filtrate, pour out the filtrate, and then continue to collect the filtrate in this beaker until the filtration is completed. A3.2.2 Pipette 25.00ml of the test solution (A3.2.1) into a 300ml conical flask and add 75ml of ethanol. Add 4~5 drops of bromocresol blue indicator. If the solution is yellow, add 1mol/L sodium hydroxide solution until it turns blue, then add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess: If the solution is blue, add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess. Add 1ml of diphenylazocarbonyl indicator to the sample solution, and titrate with a standard solution of mercuric nitrate of appropriate concentration (the titration volume of the standard solution of mercuric nitrate is controlled at 7-15ml) until the solution changes from yellow to purple-red, which is the end point. At the same time, perform a blank test. A3.3 Expression of analysis results:
The mass percentage of chloride (in terms of CI) is calculated as follows: 2c(V-Vo)×35.45
m×100
Where: C1--mass percentage of CI\, %; 100%
C——actual concentration of standard solution of mercuric nitrate, mol/L.; V-volume of standard solution of mercuric nitrate consumed by the test solution, ml; Vo-volume of standard solution of mercuric nitrate consumed by the blank test, ml; V-volume of the test solution absorbed, ml;
m-mass of the sample, g.
YYKAONrKACas
·（A2）
SJ/T11136-1997
Appendix B
（Suggested Appendix）
Treatment of waste liquid containing mercury
In order to prevent the pollution of wastewater, it is recommended to treat the waste liquid obtained after the determination of chloride by mercury titration as follows. Collect the waste liquid after the determination in a container of appropriate size (such as: 50L), precipitate mercury with excess sodium sulfide in alkaline medium, and oxidize excess sodium sulfide with hydrogen peroxide to prevent mercury from dissolving in the form of polysulfide. Operation procedure: Collect the waste liquid in a container of about 50L. When the waste liquid reaches about 40L, add 400ml 40% sodium hydroxide solution and 100g sodium sulfide nonahydrate in sequence. After 10 minutes, slowly add 400ml 30% hydrogen peroxide solution and mix thoroughly. After 24 hours, drain the upper clear liquid into the waste water and transfer the sediment to another container for mercury recovery by a dedicated person.0.5mol/L standard solution: weigh 2.9222g of standard sodium chloride that has been pre-calcined at 500℃～600℃ for 1h and cooled in a desiccator, place it in a beaker, add a small amount of water to dissolve, transfer all the solution into a 1000ml volumetric flask, add water to the scale, and shake well. bzxz.net
b) 0.001mol/L or other concentration standard solution: accurately dilute the 0.05mol/L standard solution to the required multiple. A2.7 Mercuric nitrate standard solution:
a) 0.025mol/L standard solution: weigh 8.57g mercuric nitrate [Hg(Nox)2H,O], put it in a 250ml beaker, add 7ml 1+1 nitric acid solution, add a small amount of water to dissolve and filter, transfer to a 1000ml volumetric flask, add water to the scale and shake well; b) 0.005mol/L0.001mol/L or other concentration mercuric nitrate standard solution: accurately dilute the 0.025mol/L mercuric nitrate standard solution to the required multiple. When diluting, add an appropriate amount of 1:1 nitric acid solution to prevent the hydrolysis of mercuric nitrate: c) Calibration method of 0.025mol/L, 0.005mol/L, 0.001mol/L or other concentrations of mercuric nitrate standard solution: Accurately transfer 5.00ml of the corresponding sodium chloride standard solution, place it in a conical flask, add 5ml of water, 30ml of ethanol and 2 drops of bromophenol blue indicator, and add 1mol/L nitric acid solution until the solution changes from blue to yellow, then add 2~3 drops in excess, add 1ml of benzyl azocarbonyl indicator, and titrate with the corresponding concentration of mercuric nitrate standard solution until the solution changes from yellow to purple-red, which is the end point. At the same time, perform an empty mouth test. Keep the mercury-containing waste liquid after titration and treat it according to Appendix B. The concentration of nitric acid multiplied by the standard titration solution is calculated as follows: C,x Vi
C=2(VV,)
Wherein: C is the actual concentration of the standard titration solution of mercuric nitrate, mol/L; C is the concentration of the standard titration solution of sodium chloride, mol/L; V is the volume of the standard titration solution of mercuric nitrate consumed in the titration, ml; V is the volume of the standard titration solution of mercuric nitrate consumed in the blank titration, ml. A3 Analysis steps
YKAONrKAcas
（A1)
A3.1 Test material
SJ/T11136-1997
Weigh 10g of test material (all test material grinding rates are 100 days), accurate to 0.01g. A3.2 Determination
A3.2.1 Place the sample (A3.1) in a 250ml beaker, add 100ml water, cover with a watch glass, stir every 6min, immerse for 1h, filter with double-layer filter paper, collect the filtrate in a 100ml beaker, and when the filtrate is 15ml, rinse the beaker with the filtrate, pour out the filtrate, and then continue to collect the filtrate in this beaker until the filtration is completed. A3.2.2 Pipette 25.00ml of the test solution (A3.2.1) into a 300ml conical flask and add 75ml of ethanol. Add 4~5 drops of bromocresol blue indicator. If the solution is yellow, add 1mol/L sodium hydroxide solution until it turns blue, then add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess: If the solution is blue, add 1mol/L nitric acid solution until it turns yellow, and then add 3~4 drops in excess. Add 1ml of diphenylazocarbonyl indicator to the sample solution, and titrate with a standard solution of mercuric nitrate of appropriate concentration (the titration volume of the standard solution of mercuric nitrate is controlled at 7-15ml) until the solution changes from yellow to purple-red, which is the end point. At the same time, perform a blank test. A3.3 Expression of analysis results:
The mass percentage of chloride (in terms of CI) is calculated as follows: 2c(V-Vo)×35.45
m×100
Where: C1--mass percentage of CI\, %; 100%
C——actual concentration of standard solution of mercuric nitrate, mol/L.; V-volume of standard solution of mercuric nitrate consumed by the test solution, ml; Vo-volume of standard solution of mercuric nitrate consumed by the blank test, ml; V-volume of the test solution absorbed, ml;
m-mass of the sample, g.
YYKAONrKACas
·（A2）
SJ/T11136-1997
Appendix B
（Suggested Appendix）
Treatment of waste liquid containing mercury
In order to prevent the pollution of wastewater, it is recommended to treat the waste liquid obtained after the determination of chloride by mercury titration as follows. Collect the waste liquid after the determination in a container of appropriate size (such as: 50L), precipitate mercury with excess sodium sulfide in alkaline medium, and oxidize excess sodium sulfide with hydrogen peroxide to prevent mercury from dissolving in the form of polysulfide. Operation procedure: Collect the waste liquid in a container of about 50L. When the waste liquid reaches about 40L, add 400ml 40% sodium hydroxide solution and 100g sodium sulfide nonahydrate in sequence. After 10 minutes, slowly add 400ml 30% hydrogen peroxide solution and mix thoroughly. After 24 hours, drain the upper clear liquid into the waste water and transfer the sediment to another container for mercury recovery by a dedicated person.;V-the volume of the standard titration solution of mercuric nitrate consumed by the test solution, ml; Vo-the volume of the standard titration solution of mercuric nitrate consumed by the blank test, ml; V-the volume of the absorbed test solution, ml;
m-the mass of the sample, g.
YYKAONrKACas
·(A2)
SJ/T11136-1997
Appendix B
(Suggested Appendix)
Treatment of waste liquid containing mercury
In order to prevent the pollution of wastewater, it is recommended to treat the waste liquid obtained after the determination of chloride by mercury titration as follows. Collect the waste liquid after the determination in a container of appropriate size (such as: 50L), precipitate mercury with excess sodium sulfide in an alkaline medium, and oxidize the excess sodium sulfide with hydrogen peroxide to prevent the mercury from dissolving in the form of polysulfide. Operation procedure: Collect the waste liquid in a container of about 50L. When the waste liquid reaches about 40L, add 400ml 40% sodium hydroxide solution and 100g sodium sulfide nonahydrate in sequence. After 10 minutes, slowly add 400ml 30% hydrogen peroxide solution and mix thoroughly. After 24 hours, drain the upper clear liquid into the waste water and transfer the sediment to another container for mercury recovery by a dedicated person.;V-the volume of the standard titration solution of mercuric nitrate consumed by the test solution, ml; Vo-the volume of the standard titration solution of mercuric nitrate consumed by the blank test, ml; V-the volume of the absorbed test solution, ml;
m-the mass of the sample, g.
YYKAONrKACas
·(A2)
SJ/T11136-1997
Appendix B
(Suggested Appendix)
Treatment of waste liquid containing mercury
In order to prevent the pollution of wastewater, it is recommended to treat the waste liquid obtained after the determination of chloride by mercury titration as follows. Collect the waste liquid after the determination in a container of appropriate size (such as: 50L), precipitate mercury with excess sodium sulfide in an alkaline medium, and oxidize the excess sodium sulfide with hydrogen peroxide to prevent the mercury from dissolving in the form of polysulfide. Operation procedure: Collect the waste liquid in a container of about 50L. When the waste liquid reaches about 40L, add 400ml 40% sodium hydroxide solution and 100g sodium sulfide nonahydrate in sequence. After 10 minutes, slowly add 400ml 30% hydrogen peroxide solution and mix thoroughly. After 24 hours, drain the upper clear liquid into the waste water and transfer the sediment to another container for mercury recovery by a dedicated person.
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