SJ 20637-1997 Specification for aluminum nitride powder for electronic ceramics
Some standard content:
Military Standard of the Electronic Industry of the People's Republic of China FL5970
SJ 20637-97
Specification for AIN powder for electric ceramics Issued on 1997-06-17
Implemented on 1997-10-01
Approved by the Ministry of Electronics Industry of the People's Republic of China Military Standard of the Electronic Industry of the People's Republic of China Specification for AIN powder for eleclric ceramics
Specification for AIN powder for eleclric ceramics1 Scope
1.1 Subject Content
SJ20637-97
This specification specifies the requirements, quality assurance regulations, delivery preparation, etc. for aluminum nitride powder materials for electronic ceramics. 1.2 Scope of Application
This specification applies to aluminum nitride powder materials for electronic ceramics. 。 2 Reference standards
GB 191 - 90
GB 223.1 - 81
GB581686
GB 6522 - 86
GB 6524-86
SJ/T 10551 - 94
3 Requirements
3.1 Qualification identification
Picture mark for packaging, storage and transportation
Determination of carbon content in steel and alloy
Determination of surface area of catalyst and adsorbent
Determination of bulk density of alumina powder
Determination of particle size distribution of metal powders Light transmission method Emission spectrum analysis method for impurities in lead trifluoride for electronic ceramics The aluminum nitride powder submitted in accordance with this specification shall be a qualified product after identification. 3.2 State and color
Usually, aluminum nitride powder is in fine granular form, and its color is white, gray, or gray. 3.3 Chemical composition
The chemical composition of aluminum nitride powder is shown in Table 1. Table 1 Chemical composition and content of aluminum nitride powder
Main component content
32.0-32.5
32.5 ~ 33.0
Note: Other impurities content is measured.
The Ministry of Electronics Industry of the People's Republic of China issued the main impurity content on June 17, 1997
Implemented on October 1, 1997
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3.4 Physical properties
The physical properties of aluminum nitride powder are shown in Table 2. SJ20637—97
Table 2 Physical properties of aluminum nitride powder
Particle size distribution
4 Quality assurance provisions
4.1 Inspection responsibilities
Particle size
Bulk density
Specific surface area
(Xinxiao value)
AIN single phase
Unless otherwise specified in the contract or order, the contractor shall be responsible for completing all inspections specified in this specification. If necessary, the ordering party or the superior appraisal agency has the right to inspect any inspection item described in this specification. 4.1.1 Qualification responsibility
All products must meet all requirements of Chapter 3 and Chapter 5 of this specification. The inspections specified in this specification shall become an integral part of the contractor's entire inspection system or quality outline. If the contract includes inspection requirements not specified in this specification, the contractor shall also ensure that the products submitted for acceptance meet the contract requirements. Quality consistency sampling does not allow the submission of products that are known to be defective, nor can the ordering party be required to accept defective products. 4.2 Inspection classification
The inspections specified in this specification are divided into:
a. Identification inspection;
b. Quality consistency inspection.
4.3 Environmental conditions
Unless otherwise specified, the inspections are carried out under the following standard atmospheric conditions: temperature: 15~35;
b. Relative humidity: 45%~75%:
c. Air pressure: 86~106kPao
4.4 Identification inspection
Identification inspection should be carried out before the aluminum nitride powder is officially put into production. When there are major changes in raw materials or manufacturing processes that may affect the identification inspection results, identification inspection should also be carried out. Identification inspection is also used to verify the maintenance of identification qualification. 4.4.1 Inspection location
Identification inspection should be carried out in a laboratory approved by the relevant department. 4.4.2 Inspection samples and sample size. Inspection samples shall be manufactured using equipment and processes commonly used in production. 2
SJ 20637-97
Not less than 200g of aluminum nitride powder submitted for inspection shall be randomly selected. h
4.4.3 Inspection
The items and inspection sequence of the appraisal inspection shall be as specified in Table 3. Table 3 Identification inspection
Inspection or test items
State and color
Main component content
Main impurity content
Particle size distribution
Bulk density
Specific surface areabzxZ.net
4.4.4 Unqualified judgment
Required chapter number
Inspection or test method chapter number
If the test sample passes all the inspections or tests specified in Table 3, the identification inspection is qualified; if one or more of them do not meet the requirements specified in Table 3, the identification qualification will not be granted. 4.4.5 Maintenance of identification qualification
In order to maintain the identification qualification, the contractor shall submit batch-by-batch and periodic test data every year. 4.5 Quality consistency inspection
Quality consistency inspection is divided into batch-by-batch inspection and periodic inspection. 4.5.1 Batch inspection
4.5.1.1 Inspection batch
An inspection batch consists of aluminum nitride powders with the same formula, continuously produced under basically the same conditions and submitted for inspection at the same time.
4.5.1.2 Sampling plan
The sampling method and sample quantity shall comply with the provisions of Article 4.4.2 and the corresponding test methods. 4.5.1.3 Inspection items
Article 3.2, particle size distribution in Tables 1 and 2, and loose density. 4.5.1.4 Judgment rules
When inspected according to the inspection method specified in Article 4.7 of this specification, if the indicators of all samples meet the requirements of Article 3.2 and Tables 1 and 2, the batch inspection is qualified. If one or more of the inspection results do not meet the requirements, double sampling should be taken from the batch, and the unqualified items should be re-inspected. If the re-inspection still fails, the batch of products is unqualified. 4.5.2 Periodic inspection
4.5.2.1 Inspection items and periodicity
Periodic inspection shall be carried out in accordance with the items specified in Article 3.2 and Tables 1 and 2. Periodic inspection shall not be less than once a year. When the manufacturing process or raw materials are significantly changed, periodic inspection shall also be carried out. 4.5.2.2 Sampling plan
Samples shall be taken and prepared in accordance with Article 4.4.2 and the corresponding test methods from the products that have passed the batch inspection. 4.5.2.3 Judgment rules
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SJ 2063797
When the inspection is carried out in accordance with the inspection method specified in Article 4.7 of this specification, if the indicators of all samples meet the requirements of Article 3.2 and Tables 1 and 2 of this specification, the periodic inspection is qualified. If one or more test results do not meet the requirements during the test, the unqualified items shall be re-inspected with twice the number of samples. If the re-inspection still fails, the periodic inspection is unqualified. 4.6 Packaging Inspection
The packaging and marking inspection specified in Chapter 5 of this specification shall be carried out by visual inspection. Any transport package that does not meet the requirements of Chapter 5 shall be rejected.
4.7 Inspection Method
4.7.1 State and Color
Visual inspection shall be used.
4.7.2 Main Component Content
4.7.2.1 Nitrogen Content
The determination method of nitrogen content is shown in Appendix A (Supplement). When the purchaser has requirements, the two parties shall negotiate separately. 4.7.2.2 Aluminum Content
The determination method of aluminum content is shown in Appendix B (Supplement). 4.7.3 Main Impurity Content
4.7.3.1 Oxygen Content
The oxygen content is determined by a coulometric oxygen analyzer (KLST40SA tester). 4.7.3.2 Carbon content
Carbon content shall be determined in accordance with GB223.1.
4.7.3.3 Iron and silicon content
Iron and silicon trace elements shall be determined in accordance with SI/T 10551. 4.7.4 Particle size distribution
Particle size distribution and average particle size shall be determined in accordance with the method specified in GB6524. Anhydrous alcohol and sodium hexametaphosphate shall be used as dispersants.
4.7.5 Bulk density
Bulk density shall be determined in accordance with GB 6522.
4.7.6 Specific surface area
Specific surface area shall be determined in accordance with GB5816.
4.7.7 Physical Phase
ALN phase is determined by X-ray diffraction method, and there should be no impurity peaks. 5 Delivery Preparation
5.1 Packaging
Aluminum nitride powder is packaged in plastic bottles or iron barrels sealed with plastic film, and the minimum package is 500g. 5.2 Marking
The packaging markings of aluminum nitride powder should meet the requirements of GB191 and comply with the following regulations: 5.2.1 A label should be placed in the package of aluminum nitride powder, which should indicate: a. Name of the manufacturer:
b. Product name;
c. Trademark;
d. Product grade;
SI20637-97
e. Manufacturing date (or number) or production batch number:
f. Standard number:
name. Seal of inspector.
5.2.2 The packaging of aluminum nitride powder should have the following signs; a.
Manufacturer name;
Product name;
c. Trademark;
d. Product grade;
e. Manufacturing date or production batch number
f. "Moisture-averse", "waterproof", etc.
5.3 Transportation
Aluminum nitride powder can be transported by any means of transportation, but it should be waterproof and pollution-proof. 5.4 Storage
Aluminum nitride powder should be stored in a ventilated and clean warehouse, separated from other materials, and prevented from moisture. The relative humidity (RH) should be ≤75%, the storage temperature should be ≤35C, and the storage period is half a year. If the storage period is exceeded, it should be re-inspected and can only be sold after passing the inspection. 6 Notes
6.1 Intended use
The complex aluminum powder specified in this specification is intended to be used in the production of aluminum nitride electronic ceramics, and can also be used as an additive to improve heat dissipation. 6.2 Contents of order documents
The following contents should be stated in the contract or order: 3. Name and number of this specification;
b. Grade;
c. Quantity;
d. Other information.
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Principle Summary
SJ 20637-97
Appendix A
Determination of Nitrogen Content
(Supplement)
Use phosphoric acid to heat and decompose the sample, and distill it once to determine the fluorine. The determination principle is as follows:AIN + 4H,PO. - A1(H,PO4)3 + NH,H,PO4NH,H,PO4 + 3NaOH= NH + + Na,PO4 +3H,ONH, +H,BO,= H,BO·NH
H,BO-NH, + HC1 = H,BO, + NH,C1A2 Test materials and requirements
Phosphorus-sulfur mixed acid 1:1 (wt%);
Sodium hydroxide solution 40%;
Boric acid solution 2%;
Hydrochloric acid standard solution 0.1mol/m3 (preparation and calibration adopt conventional methods in analytical chemistry); indicator PH=5,1 bromocresol green methyl red acetic acid solution. A3 Test device
The test device is shown in Figure A1.
40%NaOH
Sample solution
2% H,BO
Figure A1 Evaporation experimental device
A4 Determination operation process
SI 20637-97
a: Weigh 0.4g of the ground and dried sample accurately and place it in a 200ml beaker: b. Add 20ml of 1:1 phosphorus-sulfur mixed acid and slowly heat until the sample is completely decomposed. After cooling, transfer to a 250ml volumetric flask and dilute to full scale;
c. Accurately remove 50ml of the solution from the above volumetric flask and place it in a distilling flask: d. Assemble the distillation experimental device according to Figure A1. Add 100ml of 2% boric acid solution to the absorption flask; e. Add 100ml of 40% sodium hydroxide solution to the condenser at the upper end of the distillation flask, add it drop by drop to the distillation flask, slowly heat and distill until the nitrogen completely escapes and is absorbed, and stop distillation. r. Remove the absorption flask and add 8 drops of indicator, and drip 0.1mol/m2 hydrochloric acid until the solution changes from green to pink, which is the end point. Perform a blank test at the same time.
A5 Data processing of test results
Nitrogen content = N(V-Va)×0.014
X100% ...
G× 50/250
Aluminum nitride content = 2.926×nitrogen content (%), where; N—hydrochloric acid equivalent concentration;
Vj—--volume of hydrochloric acid used for sample, ml;
Vz——volume of hydrochloric acid used for blank test, ml; G sample weight, g:
0.014——milligram equivalent of nitrogen, mg;
2.926——conversion coefficient of nitrogen to aluminum nitride. +(1)
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B1 Principle overview
EDTA direct complexometric titration method is adopted.
B2 Experimental materials and requirements
Boric acid analytical grade;
Sodium carbonate analytical grade;
Hydrochloric acid 50%;
NaAc-HAc buffer pH=5.5;
Water 50%;
EDTA 0.05mol;
SJ20637-97
Appendix B
Determination of aluminum content
(Supplement)
Lead standard solution 0.04mol (preparation and calibration adopt conventional methods in analytical chemistry); methyl red 0.1% ethanol solution;
Xylenol 0.2%.
B3 Experimental equipment
Platinum pot;
Volume flask;
Conical flask.
B4 Test procedure
Accurately weigh 0.2g sample and place it in a platinum pot: a.
b, add appropriate amount of 1:1 boric acid and sodium carbonate solid 4g. Melt the sample at 950C for 30min; c. After cooling, soak it with water and acidify it with 1:1 hydrochloric acid, with an excess of 10ml: d, transfer it to a 250ml volumetric flask and dilute it to full scale; transfer 50ml of this solution to a 250ml conical flask, add 0.05malEDTA25rml and heat to about 80C, e
Use 1:1 ammonia water to adjust the solution from red to yellow: then add 15ml of buffer solution, heat and boil for 2~3min, and add 5 drops of xylenol orange after cooling; then add lead acetate standard solution until the solution changes from yellow to red, which is the end point. B5 Data processing of test results
(MV,-MV2)×0.02698
Total aluminum content=
G×50/250
Wherein; M—molar concentration of lead acetate solution: V.-
Volume of lead acetate solution consumed by blank, ml; Vvolume of lead acetate solution consumed by sample, ml; 8
G—sample weight, gi
0.02698—milligram equivalent of aluminum, mg.
Note: When the impurity content is high, a concealing agent should be used. Additional remarks:
SI 20637-97
This specification is under the jurisdiction of the China Institute of Electronics Technology. This specification was drafted by the 43rd Institute of the Ministry of Electronics Industry. The main drafters of this specification: Xu Dongsheng, Huang Anbing, Cui Zang, Lei Jian, Feng Youmin. Project code: B5509.
TTKAONTKAca-2. Contents of order documents
The following contents shall be stated in the contract or order:3. Name and number of this specification;
b. Level;
c. Quantity;
d. Other information.
KAONKAca-
Principle Summary
SJ 20637-97
Appendix A
Determination of nitrogen content
(Supplement)
Use phosphoric acid to heat and decompose the sample, and distill it once to determine the fluorine. The determination principle is as follows: AIN + 4H,PO. - A1(H,PO4)3 + NH,H,PO4NH,H,PO4 + 3NaOH = NH + + Na,PO4 +3H,ONH, +H,BO, = H,BO·NH
H,BO-NH, + HC1 = H,BO, + NH,C1A2 Test materials and requirements
Phosphorus and sulfur mixed acid 1:1 (wt%);
Sodium hydroxide solution 40%;
Boric acid solution 2%;
Hydrochloric acid standard solution 0.1mol/m3 (preparation and calibration adopt conventional methods in analytical chemistry); Indicator PH = 5,1 bromocresol green methyl red acetic acid solution. A3 Test device
The test device is shown in Figure A1.
40%NaOH
Sample solution
2% H,BO
Figure A1 Evaporation experiment device
A4 Determination operation process
SI 20637-97
a: Accurately weigh 0.4g of ground and dried sample and place it in a 200ml beaker: b, add 20ml of 1:1 phosphorus-sulfur mixed acid and slowly heat until the sample is completely decomposed. After cooling, transfer to a 250ml volumetric flask and dilute to full scale;
c. Accurately transfer 50ml of solution from the above volumetric flask and place it in a steaming bottle: d. Assemble the distillation experiment device according to Figure A1. Add 100ml of 2% boric acid solution to the absorption bottle; e. Add 100ml of 40% sodium hydroxide solution to the condenser at the top of the distillation bottle, add it drop by drop to the distillation bottle, slowly heat and distill until the nitrogen completely escapes and is absorbed, stop distillation r. Remove the absorption bottle and add 8 drops of indicator, add 0.1mol/m2 hydrochloric acid until the solution changes from green to pink, which is the end point. At the same time, carry out a blank test.
A5 Data processing of test results
Nitrogen content = N(V-Va)×0.014
X100% ...
G× 50/250
Aluminum nitride content = 2.926×nitrogen content (%), where; N—hydrochloric acid equivalent concentration;
Vj—--volume of hydrochloric acid used for sample, ml;
Vz——volume of hydrochloric acid used for blank test, ml; G sample weight, g:
0.014——milligram equivalent of nitrogen, mg;
2.926——conversion coefficient of nitrogen to aluminum nitride. +(1)
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B1 Principle overview
EDTA direct complexometric titration method is adopted.
B2 Experimental materials and requirements
Boric acid analytical grade;
Sodium carbonate analytical grade;
Hydrochloric acid 50%;
NaAc-HAc buffer pH=5.5;
Water 50%;
EDTA 0.05mol;
SJ20637-97
Appendix B
Determination of aluminum content
(Supplement)
Lead standard solution 0.04mol (preparation and calibration adopt conventional methods in analytical chemistry); methyl red 0.1% ethanol solution;
Xylenol 0.2%.
B3 Experimental equipment
Platinum pot;
Volume flask;
Conical flask.
B4 Test procedure
Accurately weigh 0.2g sample and place it in a platinum pot: a.
b, add appropriate amount of 1:1 boric acid and sodium carbonate solid 4g. Melt the sample at 950C for 30min; c. After cooling, soak it with water and acidify it with 1:1 hydrochloric acid, with an excess of 10ml: d, transfer it to a 250ml volumetric flask and dilute it to full scale; transfer 50ml of this solution to a 250ml conical flask, add 0.05malEDTA25rml and heat to about 80C, e
Use 1:1 ammonia water to adjust the solution from red to yellow: then add 15ml of buffer solution, heat and boil for 2~3min, and add 5 drops of xylenol orange after cooling; then add lead acetate standard solution until the solution changes from yellow to red, which is the end point. B5 Data processing of test results
(MV,-MV2)×0.02698
Total aluminum content=
G×50/250
Wherein; M—molar concentration of lead acetate solution: V.-
Volume of lead acetate solution consumed by blank, ml; Vvolume of lead acetate solution consumed by sample, ml; 8
G—sample weight, gi
0.02698—milligram equivalent of aluminum, mg.
Note: When the impurity content is high, a concealing agent should be used. Additional remarks:
SI 20637-97
This specification is under the jurisdiction of the China Institute of Electronics Technology. This specification was drafted by the 43rd Institute of the Ministry of Electronics Industry. The main drafters of this specification: Xu Dongsheng, Huang Anbing, Cui Zang, Lei Jian, Feng Youmin. Project code: B5509.
TTKAONTKAca-2. Contents of order documents
The following contents shall be stated in the contract or order:3. Name and number of this specification;
b. Level;
c. Quantity;
d. Other information.
KAONKAca-
Principle Summary
SJ 20637-97
Appendix A
Determination of nitrogen content
(Supplement)
Use phosphoric acid to heat and decompose the sample, and distill it once to determine the fluorine. The determination principle is as follows: AIN + 4H,PO. - A1(H,PO4)3 + NH,H,PO4NH,H,PO4 + 3NaOH = NH + + Na,PO4 +3H,ONH, +H,BO, = H,BO·NH
H,BO-NH, + HC1 = H,BO, + NH,C1A2 Test materials and requirements
Phosphorus and sulfur mixed acid 1:1 (wt%);
Sodium hydroxide solution 40%;
Boric acid solution 2%;
Hydrochloric acid standard solution 0.1mol/m3 (preparation and calibration adopt conventional methods in analytical chemistry); Indicator PH = 5,1 bromocresol green methyl red acetic acid solution. A3 Test device
The test device is shown in Figure A1.
40%NaOH
Sample solution
2% H,BO
Figure A1 Evaporation experiment device
A4 Determination operation process
SI 20637-97
a: Accurately weigh 0.4g of ground and dried sample and place it in a 200ml beaker: b, add 20ml of 1:1 phosphorus-sulfur mixed acid and slowly heat until the sample is completely decomposed. After cooling, transfer to a 250ml volumetric flask and dilute to full scale;
c. Accurately transfer 50ml of solution from the above volumetric flask and place it in a steaming bottle: d. Assemble the distillation experiment device according to Figure A1. Add 100ml of 2% boric acid solution to the absorption bottle; e. Add 100ml of 40% sodium hydroxide solution to the condenser at the top of the distillation bottle, add it drop by drop to the distillation bottle, slowly heat and distill until the nitrogen completely escapes and is absorbed, stop distillation r. Remove the absorption bottle and add 8 drops of indicator, add 0.1mol/m2 hydrochloric acid until the solution changes from green to pink, which is the end point. At the same time, carry out a blank test.
A5 Data processing of test results
Nitrogen content = N(V-Va)×0.014
X100% ...
G× 50/250
Aluminum nitride content = 2.926×nitrogen content (%), where; N—hydrochloric acid equivalent concentration;
Vj—--volume of hydrochloric acid used for sample, ml;
Vz——volume of hydrochloric acid used for blank test, ml; G sample weight, g:
0.014——milligram equivalent of nitrogen, mg;
2.926——conversion coefficient of nitrogen to aluminum nitride. +(1)
YKAONKAca-
B1 Principle overview
EDTA direct complexometric titration method is adopted.
B2 Experimental materials and requirements
Boric acid analytical grade;
Sodium carbonate analytical grade;
Hydrochloric acid 50%;
NaAc-HAc buffer pH=5.5;
Water 50%;
EDTA 0.05mol;
SJ20637-97
Appendix B
Determination of aluminum content
(Supplement)
Lead standard solution 0.04mol (preparation and calibration adopt conventional methods in analytical chemistry); methyl red 0.1% ethanol solution;
Xylenol 0.2%.
B3 Experimental equipment
Platinum pot;
Volume flask;
Conical flask.
B4 Test procedure
Accurately weigh 0.2g sample and place it in a platinum pot: a.
b, add appropriate amount of 1:1 boric acid and sodium carbonate solid 4g. Melt the sample at 950C for 30min; c. After cooling, soak it with water and acidify it with 1:1 hydrochloric acid, with an excess of 10ml: d, transfer it to a 250ml volumetric flask and dilute it to full scale; transfer 50ml of this solution to a 250ml conical flask, add 0.05malEDTA25rml and heat to about 80C, e
Use 1:1 ammonia water to adjust the solution from red to yellow: then add 15ml of buffer solution, heat and boil for 2~3min, and add 5 drops of xylenol orange after cooling; then add lead acetate standard solution until the solution changes from yellow to red, which is the end point. B5 Data processing of test results
(MV,-MV2)×0.02698
Total aluminum content=
G×50/250
Wherein; M—molar concentration of lead acetate solution: V.-
Volume of lead acetate solution consumed by blank, ml; Vvolume of lead acetate solution consumed by sample, ml; 8
G—sample weight, gi
0.02698—milligram equivalent of aluminum, mg.
Note: When the impurity content is high, a concealing agent should be used. Additional remarks:
SI 20637-97
This specification is under the jurisdiction of the China Institute of Electronics Technology. This specification was drafted by the 43rd Institute of the Ministry of Electronics Industry. The main drafters of this specification: Xu Dongsheng, Huang Anbing, Cui Zang, Lei Jian, Feng Youmin. Project code: B5509.
TTKAONTKAca-5;
Water 50%;
EDTA 0.05mol;
SJ20637-97
Appendix B
Determination of aluminum content
(Supplement)
Lead standard solution 0.04mol (preparation and calibration adopt conventional methods in analytical chemistry); methyl red 0.1% ethanol solution;
Xylenol 0.2%.
B3 Experimental equipment
Platinum pot;
Volume flask;
Conical flask.
B4 Test procedure
Accurately weigh 0.2g sample and place it in a platinum pot: a.
b, add appropriate amount of 1:1 boric acid and sodium carbonate solid 4g. Melt the sample at 950C for 30min; c. After cooling, soak it with water and acidify it with 1:1 hydrochloric acid, with an excess of 10ml: d, transfer it to a 250ml volumetric flask and dilute it to full scale; transfer 50ml of this solution to a 250ml conical flask, add 0.05malEDTA25rml and heat to about 80C, e
Use 1:1 ammonia water to adjust the solution from red to yellow: then add 15ml of buffer solution, heat and boil for 2~3min, and add 5 drops of xylenol orange after cooling; then add lead acetate standard solution until the solution changes from yellow to red, which is the end point. B5 Data processing of test results
(MV,-MV2)×0.02698
Total aluminum content=
G×50/250
Wherein; M—molar concentration of lead acetate solution: V.-
Volume of lead acetate solution consumed by blank, ml; Vvolume of lead acetate solution consumed by sample, ml; 8
G—sample weight, gi
0.02698—milligram equivalent of aluminum, mg.
Note: When the impurity content is high, a concealing agent should be used. Additional remarks:
SI 20637-97
This specification is under the jurisdiction of the China Institute of Electronics Technology. This specification was drafted by the 43rd Institute of the Ministry of Electronics Industry. The main drafters of this specification: Xu Dongsheng, Huang Anbing, Cui Zang, Lei Jian, Feng Youmin. Project code: B5509.
TTKAONTKAca-5;
Water 50%;
EDTA 0.05mol;
SJ20637-97
Appendix B
Determination of aluminum content
(Supplement)
Lead standard solution 0.04mol (preparation and calibration adopt conventional methods in analytical chemistry); methyl red 0.1% ethanol solution;
Xylenol 0.2%.
B3 Experimental equipment
Platinum pot;
Volume flask;
Conical flask.
B4 Test procedure
Accurately weigh 0.2g sample and place it in a platinum pot: a.
b, add appropriate amount of 1:1 boric acid and sodium carbonate solid 4g. Melt the sample at 950C for 30min; c. After cooling, soak it with water and acidify it with 1:1 hydrochloric acid, with an excess of 10ml: d, transfer it to a 250ml volumetric flask and dilute it to full scale; transfer 50ml of this solution to a 250ml conical flask, add 0.05malEDTA25rml and heat to about 80C, e
Use 1:1 ammonia water to adjust the solution from red to yellow: then add 15ml of buffer solution, heat and boil for 2~3min, and add 5 drops of xylenol orange after cooling; then add lead acetate standard solution until the solution changes from yellow to red, which is the end point. B5 Data processing of test results
(MV,-MV2)×0.02698
Total aluminum content=
G×50/250
Wherein; M—molar concentration of lead acetate solution: V.-
Volume of lead acetate solution consumed by blank, ml; Vvolume of lead acetate solution consumed by sample, ml; 8
G—sample weight, gi
0.02698—milligram equivalent of aluminum, mg.
Note: When the impurity content is high, a concealing agent should be used. Additional remarks:
SI 20637-97
This specification is under the jurisdiction of the China Institute of Electronics Technology. This specification was drafted by the 43rd Institute of the Ministry of Electronics Industry. The main drafters of this specification: Xu Dongsheng, Huang Anbing, Cui Zang, Lei Jian, Feng Youmin. Project code: B5509.
TTKAONTKAca-
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