GB/T 5070.8-2002 Chemical analysis methods for magnesia-chromium refractories Part 8: CyDTA volumetric method for determination of magnesium oxide content
Some standard content:
National Standard of the People's Republic of China
CB/T 5070.1~5070.12—2002
tReplacement of Gn/T nn.1.~0?.13- 19s
Chemical analysis of magnesia chromitc refractorics2002-1231Promulgated by General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
20030601Implementation
TCS B1.080
National Standard of the People's Republic of China
GB/T 5070,8-2002
GH/T 5(0.7--193
Chemical analysis of magnesia chromite refractories-Part 8: Determination of magnesium oxide CyDTA volumetric methodChemical analysis of magoesia chromite refractories-Part 8: Determination of magnesium oxide CyDTA volumetric method: methodPublished on 2002-12-31
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
Implementation on 2003-06-01
GB/T 5070.8—2002
GB/T5373.3 The methods for analysis of fire materials are divided into several parts: Part 1: Determination of loss on ignition; Part 2: Photometric determination of lead ions; Part 3: Determination of iron hydride by EDTA method; Part 4: Determination of chemical content by EDTA method; Part 5: Determination of chemical content by ECTA method; Part 6: Determination of hydrogenation by volume; Part 7: Part T: Determination of the content of calcium oxide by volumetric method: Part 8: Determination of the content of magnesium oxide by CyDTA volumetric method: Part 10: Determination of the content of dichromate by titanium dioxide mass spectrometry: Part 12: Determination of the content of sodium monoxide by pyrolysis: Part 13: Determination of the content of sodium monoxide by pyrolysis: Part 14: Determination of the content of sodium monoxide by pyrolysis: Part 15: Determination of the content of sodium monoxide by pyrolysis: Part 16: Determination of the content of sodium monoxide by pyrolysis: Part 17: Determination of the content of sodium monoxide by pyrolysis: Part 18: Determination of the content of sodium monoxide by pyrolysis: Part 19: Determination of the content of sodium monoxide by pyrolysis: Part 20: Determination of the content of sodium monoxide by pyrolysis: Part 21: Determination of the content of sodium monoxide by pyrolysis: Part 22: Determination of the content of sodium monoxide by pyrolysis: Part 23: Determination of the content of sodium monoxide by pyrolysis: Part 24: Determination of the content of sodium monoxide by pyrolysis: Part 25: Determination of the content of sodium monoxide by pyrolysis: Part 26: Determination of the content of sodium monoxide by pyrolysis: Part 27: Determination of the content of sodium monoxide by pyrolysis: Part 28: Determination of the content of sodium monoxide by pyrolysis: Part 29: Determination of the content of sodium monoxide by pyrolysis: Part 30: Determination of the content of sodium monoxide by pyrolysis: Part 31: Determination of the content of sodium monoxide by pyrolysis: Part 32: Determination of the Standardization of chemical analysis methods for refractory materials. This part has the following main changes compared with GB/E07C.2-985: - "Foreword", "Supplementary References", "Quality Assurance and Confidentiality", and "Test Report" are added; - Detailed provisions are made on sample preparation to increase operability; - Provisions on the selection of analytical parameters are added, and other specifications are allowed; - The sample range of 0.508 is changed to 0.5e for the purpose of drying and melting; - Determination of oxygen by CyLTA mask method t||—CB/T507).Y—198ECy)TA standard titration liquid swells greatly, the wood will adjust (CTA) = Q,0>moJ to (C Ting A) U.35m/1. The titration is carried out to reduce the alcohol content. According to (I3/T1.13000 "International Standardization Guidelines for L. Part: Standard Structure and Contraction Rules and H/20092.420019 Standard Writing Rules Part 4, the chemical analysis method is also a standard reduction.
This part is issued by the former National Tourism Standardization Institute of Gold Industry. This part is issued by the National Technical Committee for International Standardization of Refractory Materials (CSHS/TC93) and is drafted by: Jiyang Refractory Research Institute, Anshan Metallurgical Geological Exploration Company. This part was drafted by: Guo Yihong, Liang Zai, Gongzhen Institute. The current version of the standard replaced by this part is: GB/T 5070.71585.
1 Scope
Chemical analysis methods for magnesia-chromium refractories
Part 8: Determination of magnesium oxide content by CDTA volumetric method This part of GB/T 5070.71585 specifies the method for determining magnesium hydride content by CDTA volumetric method: GB/T 5970.8—2002
This part is applicable to the determination of magnesium hydride content in chromium-chromium refractories. The determination range (volume fraction) is 33.20-96.005% 2 Normative references
The following clauses become part of GB/T 5070.71585 by reference in this part of GB/T 5070.71585. For the recording of this part, any dated reference accompanied by all subsequent amendments (not including errata or revisions) does not apply to this part. However, the parties to this part shall consider whether the latest version of these documents can be used. The latest version of the referenced documents shall apply to all three parts.
13/T51.1202 Chemical analysis of magnesium-chromium pyrotechnic materials Part 1: Determination of power supply environment GHT17F efficiency value dream about current rules
5 Determination of heat absorption age of pyrotechnic products on the market
GB/T10325
GHT 128C5
GB/T12
GB/T1280
Experimental military technology instrument Pu Ding tube
Real transmission room or frequency instrument single mark line container or system
Laboratory glass controller
Single mark line pipette
B Refractory raw materials use amorphous pre-refractory materials to take details 3 principles
Sincerity with pregnancy Jun hook period sleep mixed a culture agent through melting, hydrochloric acid did not take a month ethyl ion reduction high price fall with six times dry base training building "precipitation separation iron, aluminum money, etc., take part of the filtrate, add premature with TA Lao Bi et al. used the acid blue K-phenol green 1 filtrate as the aging indicator. Use 1) TA standard test solution to determine the end point when the color of the droplet turns blue: 4 Reagents and instruments
4.1 Mix phosphating agent Take 1 part of sodium phosphate and 1 part of sodium phosphate in running water, grind it into fine powder, and add 4.2 Chemical reaction (300): 4.3 Hydrogen peroxide solution (3006/13.4.4 Government use 101.).
4.5 Hydrogen peroxide solution ([=u]) Weigh 37.5 parts of chlorinated water. Add 570 ml oxygen water (3.9g/water diluted to [000ml.. Mix.
4.8 Art group.
4.97. Original flow (1+1).
4.10 EGA grid wave 3.1 Weigh the R alcohol: can gel H degree (ETA) Yi00m olefins. Add 2. water, low silver heating, filter and drop potassium oxide drop liquid (.2) ≤ case can cool single year temperature, transfer to U). capacity to medium, use dilute to most degrees, pain spoon.
GB/T5070.8-2CC2
4.11 Chemical money Standard solution L.Mg-0.025r.o1/weigh 0.503$ Yan first stored in 955--332 and 1 bath cooled to temperature of the oxidation (9.9, 10 25r1 cup, add a little water, add 14.6-3L salt solution back to the cup, heat and boil, sieve to dissolve, cool and wet, transfer to 50r: container (4.16) with dilution rate scale, 4.12 (TA standard titration technique [(CyTA) 5.325mo.1]: 4.12.1 preparation
weigh 1 more! Heat the oxidizing agent (4.2) in a 25 ml beaker until just heated, remove it, cool it to room temperature, transfer it to a second volumetric flask, dilute the sample with H2O to the mark, and separate it into 4.12.2 Calibration. Use a sterilizing tube (1.17) to take 3 portions of 70.30 ml of the oxidizing agent (4.111) and place them in 400 beakers, about 1 cm3, add 2 drops of chromium blue K indicator (4.14) and (acid green indicator 4.15) and titrate with a standard titration solution (4.2). When the blue red color disappears and turns blue-green, the titration is complete. When the DTA reaches 10% of the titration volume (m3), calculate the average volume V. Then, it should be recalibrated. 4.12.3 The accuracy of the CT standard titration solution is calculated by the formula: (CyDTA)-V)--the concentration of magnesium chloride standard solution. The unit is L liter (m/T), V,--the effective value of the volume of magnesium chloride base solution (4.11) removed, the unit is (raE): - the effective value of the half-average oxidation loss (y) of the TA standard titration rate (4.12). The four-digit formula is used to judge the accuracy of the CT standard titration solution.
4.13 Congo red test line,
4.14 Acid performance test box solution (/1, triethanolamine solution (1) preparation 4. 15. The filter of the risk indicator group (5 g/L) is prepared with 1-ethylamine solution (1 + 1). 4.18. Pipette: GB/T12835 Class A.
4.17. Full-fill tube: G/12453 Class A,
4.19. Container: GB:T23:15 Class A.
5 Sample
5. 1 Sampling procedure
According to G/J25 and BT17617, collect the experimental sample. 5.2 Sample preparation
According to GB/T5070,1-2002. 5.2 Preparation
6 Analysis procedure
6.1 Number of determinations
Specify under its renaturation conditions? times.
0.2 Sample amount
Pipette about 3.20 μg and make sure to add 1 μg:
6.3 Blank test
Perform a blank test under normal conditions,
6.4 Verification test
Analyze the same standard substance with the sample under the same renaturation conditions. 6.5 Determination
TB/T 5C70.3—2002
6.5.1 Place the sample in a flask containing 3 g of the combined flux (4.1) and remove the lid. Place the mixture in a 0.05-9.00 °C furnace and heat to 1000 °C for 15 min to 30 min. Remove the sample and allow the molten material to adhere evenly to the flask and cool. 6.5.2 Clean the outer wall of the flask with filter paper and add 30 mL of acid (4.1) and 5 mL of water in a beaker. Add 1 mL of hot water. Set the melt to the point of dissolution with hot acid (.7> wash out and cover with 121\1. alcohol (1.A). Cool to room temperature. 6.5.3 Add a small piece of Congo test sample 4.13) to the solution. Use potassium peroxide solution (4.2) to neutralize most of the age (the red test paper is blue-purple). Add 1 methyl sulfoxide solution (3) until the flow precipitate appears (with the test paper red) 20%, keep at about 75min-10min
6.5.4 Filter the precipitate with medium-speed qualitative filter paper, wash with hot tetramine solution 4.11 twice, and precipitate 5 times: drain the liquid and use SL container to press.
6.5.5 Open the paper and stick it to the wall of the original beaker. Dissolve the difference with 10m hydrochloric acid (4.6), wash the filter paper with hot hydrochloric acid (1.7), dilute with water to a volume of about 150nI, cool to room temperature. 6.5.6 Neutralize the solution with 14.3l of tetramethylenetetramine solution to produce an excess of 15mT. Keep warm in the solution for 10min,
6.5. Filter with the filter paper mentioned above, rinse, filter well, cool to room temperature, adjust to the measuring point with water, and mix well. This solution is the real solution and can be used for R analysis.
6.6.B Use a pipette (4.16) to transfer 1 Cc.99 ml of test solution into 00 mL of flask. Add about 15 ml of water with a temperature of 90 °C) and stir gently. Add 10 ml of a diffuse solution (45 °C) and a positive amount of ET4 (10 °C). Add 3 drops of acid K solution (1.11) until the final solution is small (3 ml excess). Titrate until the test solution turns green. The end point is: Calculation of analytical results
7.1 The mass fraction of magnesium oxide (Mg) is expressed in %, and is calculated according to the formula: WMRO) -C: V, V1/100M x10
Wu Zhong:
V.—The numerical value of the volume of yL)TA standard titration solution (I2) consumed by the titration test wave, the unit is ml m:.): V: The numerical value of the volume of y1)1A standard titration solution (.12) consumed by the titration blank test filter, the unit is ml 1)【)1A The concentration of the standard titration wave is eliminated. The unit is rate Lml" per minute (mnl/T), the mass value of the test sample, the unit is
M——The mass value of Mg. The unit is gram year rate [year (g/1.)M=43.3117.2 points. The validity of the derivative value depends on whether the analytical value of the standard substance analyzed under the re-analysis conditions is consistent with the standard value. When the difference between the standard value and the standard value is not greater than the allowable difference, the sample analysis is valid; otherwise, it is invalid. 7.3 When the results obtained do not meet the allowable difference specified in Table 1, the arithmetic mean shall be used as the final analysis result: the test result shall be reported. The specification of Appendix A is to avoid the use of the spreadsheet and data processing. 7.2 The obtained result (H17\) shall be rounded to two decimal places. If there are requirements in the supply contract or relevant standards, the required number of digits may be rounded to the required number of digits.
8 Allowable difference
In the work, the difference between the two test results shall not be greater than the allowable difference listed in Table 1 below, 5i
CB/T 5070.S—2C02
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D Quality Assurance and Control
According to 1 heat verification
Under normal conditions, the temperature of the combustion filter should be recalibrated every two months. If the temperature inside the filter is 109.2
, the temperature should be recalibrated in time.
Test report
The test report should include the following contents:
To entrust the unit,
Name of the combat team,
An external analysis report:
Use the standard.-2
The difference between the new steps of the test (if necessary): The conduction phenomenon observed during the test (if necessary):-Test date
Conducted,
Tal z=1:
Conducted,*.
T一,2, 4,+, the national maximum value of the new value: the listed points of the "Normative Appendix!" The value of the collection analysis process is ≤1.2. GBT 5070.8-20021. The amount of magnesium oxide is expressed as mass fraction Mg. The value is expressed as % and is calculated according to the formula: WMRO) -C: V, V1/100M x10
Wu Zhong:
V.-The value of the volume of yL)TA standard titration solution (I2) consumed by the titration test wave, the unit is milliliter m:.); V: The value of the volume of y1)1A standard titration solution (.12) consumed by the titration blank test filter, the unit is milliliter 1)【)1A The concentration of the standard titration wave is eliminated. The unit is rate Lml" per minute (mnl/T), the mass value of the test sample is
M-The mass value of Mg. The unit is gram year rate [year (g/1.) M=43.3117.2 points. The validity of the derivative value depends on whether the analytical value of the standard substance analyzed under the re-analysis conditions is consistent with the standard value. When the difference between the standard value and the standard value is not greater than the allowable difference, the sample analysis is valid; otherwise, it is invalid. 7.3 When the results obtained do not meet the allowable difference specified in Table 1, the arithmetic mean shall be used as the final analysis result: the test result shall be reported. The specification of Appendix A is to avoid the use of the spreadsheet and data processing. 7.2 The obtained result (H17\) shall be rounded to two decimal places. If there are requirements in the supply contract or relevant standards, the required number of digits may be rounded to the required number of digits.
8 Allowable difference
In the work, the difference between the two test results shall not be greater than the allowable difference listed in Table 1 below, 5i
CB/T 5070.S—2C02
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D Quality Assurance and Control
According to 1 heat verification
Under normal conditions, the temperature of the combustion filter should be recalibrated every two months. If the temperature inside the filter is 109.2
, the temperature should be recalibrated in time.
Test report
The test report should include the following contents:
To entrust the unit,
Name of the combat team,
An external analysis report:
Use the standard.-2
The difference between the new steps of the test (if necessary): The conduction phenomenon observed during the test (if necessary):-Test date
Conducted,
Tal z=1:
Conducted,*.
T一,2, 4,+, the national maximum value of the new value: the listed points of the "Normative Appendix!" The value of the collection analysis process is ≤1.2. GBT 5070.8-20021. The amount of magnesium oxide is expressed as mass fraction Mg. The value is expressed as % and is calculated according to the formula: WMRO) -C: V, V1/100M x10
Wu Zhong:
V.-The value of the volume of yL)TA standard titration solution (I2) consumed by the titration test wave, the unit is milliliter m:.); V: The value of the volume of y1)1A standard titration solution (.12) consumed by the titration blank test filter, the unit is milliliter 1)【)1A The concentration of the standard titration wave is eliminated. The unit is rate Lml" per minute (mnl/T), the mass value of the test sample is
M-The mass value of Mg. The unit is gram year rate [year (g/1.) M=43.3117.2 points. The validity of the derivative value depends on whether the analytical value of the standard substance analyzed under the re-analysis conditions is consistent with the standard value. When the difference between the standard value and the standard value is not greater than the allowable difference, the sample analysis is valid; otherwise, it is invalid. 7.3 When the results obtained do not meet the allowable difference specified in Table 1, the arithmetic mean shall be used as the final analysis result: the test result shall be reported. The specification of Appendix A is to avoid the use of the spreadsheet and data processing. 7.2 The obtained result (H17\) shall be rounded to two decimal places. If there are requirements in the supply contract or relevant standards, the required number of digits may be rounded to the required number of digits.
8 Allowable difference
In the work, the difference between the two test results shall not be greater than the allowable difference listed in Table 1 below, 5i
CB/T 5070.S—2C02
3c.c3...55. Uy
SU,CI...E3.9
D Quality Assurance and Control
According to 1 heat verification
Under normal conditions, the temperature of the combustion filter should be recalibrated every two months. If the temperature inside the filter is 109.2
, the temperature should be recalibrated in time.
Test report
The test report should include the following contents:
To entrust the unit,
Name of the combat team,
An external analysis report:
Use the standard.-2
The difference between the new steps of the test (if necessary): The conduction phenomenon observed during the test (if necessary):-Test date
Conducted,
Tal z=1:
Conducted,*.
T一,2, 4,+, the national maximum value of the new value: the listed points of the "Normative Appendix!" The value of the collection analysis process is ≤1.2. GBT 5070.8-2002
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