GB/T 5070.10-2002 Chemical analysis methods for magnesia-chromium refractories Part 10: Determination of chromium trioxide content by ammonium ferrous sulfate volumetric method
Some standard content:
ICS 1. aS
National Standard of the People's Republic of China
GB/T 5070. 1~5070.12—2002
Replaces GB/T5#73.1---50V0.10-1585 Chemical analysis of magnesia chromite refracluries2002-12-31 Issued
People's Republic of China
General Administration of Quality Supervision, Inspection and Quarantine
2003-06-01 Implementation
IC551.080
Shandong National Standard
CB/T507010--2002
Chemical analysis of magnesia-chromite refractories-Part 10.Determination of chromium oxide-Annonium ferrous sufatc wolunetric Method 2002-1231 issued
People's Republic of China
with the State Administration of Quality Supervision, Inspection and Quarantine
2003-06-01 implementation
GR/T5070.10-2002
T0?0 The chemical analysis method of money network should be divided into the following parts: Part 1: Re-plate method for burning reduction: Part 2: Platinum monitoring method for determination of dihydrogen fluoride content! Part 3: Ortho-dihydrochloride method for determination of gold chloride: Part 1: EDTA content of the most legal emulsification: Part 1: Dihydrogen fluoride method for determination of iodine content: Part 2: Aluminum oxide method for determination of calcium carbonate content! Part 7: Determination of oxide content by FITA mass method; Part 1: Determination of magnesium oxide content by CDTA mass method; Part 9: Determination of oxide content by ELTA mass method; Part 10: Determination of tri-chloride content by solubility method; Part 11: Determination of oxide content by atomic absorption spectrometry; Part 12: Determination of potassium oxide by atomic absorption spectrometry. This part is part 10 of GH/15373. Part 6 replaces CB/T517\.813 magnesium station refractory material chemical composition determination method of three-way gasification:
Compared with GBT5070.81335, this part has important changes, such as: adding "Abstract", "Normative References", "Quality Assurance and Preparation", "Test Report" and making detailed provisions on sample preparation. Increased volatility; - Added the number of digits for the standard value. And allowed the other provisions: the standard range is changed from 5.00%--25. (0%\ is, 00%~50.00%": GB1.1-200C marking code Part 1: The standard structure part is compiled, that is, G12J-.1-0U standard compilation rules Part 4, the chemical composition of the position of the familiar This part is a standard for the determination of the content of chromium trioxide and chromium ions in magnesia chromium refractories. This part is a standard for the determination of the content of chromium trioxide and chromium ions in magnesia chromium refractories. This part is a standard for the determination of the content of chromium trioxide and chromium ions in magnesia chromium refractories. The method of determining the oxidation of the tree through the plate selection, the determination of the amount of three-dimensional chromium in the refractory material of magnesium chromium: determination of the release (mass fraction) is 1.00~52.00%
2 Normative references
The following clauses in the text become the subject of this part through reference to the wood part of / 5070: For any dated application document, all subsequent fuel modification orders (excluding the content of the survey) or sub-editions are not applicable to this part. However, the parties who have reached an agreement based on this part are encouraged to study whether the latest versions of these documents can be used. For any undated application document, the latest version applies to this part.
GB/T5170.1-2003 Chemical analysis methods for refractory materials of mirror-like refractory materials Part 1: Gravimetric method for loss on ignition GTR170 Rounding off rules for values
(/T10325 Sampling and acceptance criteria for shaped refractory products GB/T12305
Experimental procedures for glassware
GB/T12805 Experimental procedures for glassware
GB/T12808
(P/T17617 Sampling of refractory raw materials and unshaped refractory materials 3 Principle
The sample is mixed with magnetic acid and sodium sulfonate as a flux, and the aldehyde is taken out. In the presence of silver nitrate, lead is oxidized with persulfate. Add persulfate as an indicator and titrate to the stop point with potassium persulfate standard solution. 4 Test and Instruments
4.1 Standard Fusion Test: Grind 2 parts of hydrochloric acid and 1 part of boric acid, 4.2 Mineral silver (10 g/L).
4.3 Sulfuric acid (MnSO) (10 g/L,
4.4 Persulfate (250 g/L)
4.5 Sodium hydroxide (100 g/L).
4.6 Sulfuric acid-phosphorus acid mixture: Slowly inject 50 ml of sulfuric acid into 0.1 ml of water under constant stirring, then add 15 ml of phosphorus to mix.
4.7 Acid (21).
4.B Potassium dichromate standard solution_c (176K, Cz (,) = .35mol/L1: weigh 2.45.5g of pre-prepared heavy brand (99.99%) at 150℃~-170℃ for 2h and cool in a desiccator, add to 500ml of water, put into a 100ml volumetric flask (4.15) and add water to the scale, report sentence
4,9 teaching iron standard standard HFe (S, 5mol6?
GB/T5070,10-2002
4.9.1 Preparation
weigh 20g of ammonium sulfate [H0·(NHS06H0) containing 10mL of acid (= .71 dilute the solution with water and take 1300tnl. Evenly mix and titrate.
4.9.2 Calibration
4.9.2.1 Take 3 portions of 25 and 33mL of tantalum standard solution (4.9) in the same titration (4, 12) and place them in 400ml beakers respectively. Add 200mL of water, 20mL of tantalum (4.7), 15mL of tantalum-phosphoric acid mixed solution (4.6), 1, 2, ... , 1, calculate its average volume V, otherwise, the new standard should be reviewed:
4.9.2.2 Use a titrator (t, 12) to transfer 1,000ml. Ferrous sulfate standard solution (4.9), put it in a 400mL beaker, add 20)ml water, 2ml mercaptoaldehyde (4.7), 15ml acid-phosphoric acid mixed solution (1.6), 0.5ml monoaniline sulfonated sodium powder (4.0). Use 1)ml semi-micro titration tube (4.12) to titrate with potassium chromate standard solution (.8) until the measuring solution shows a fixed purple-red color, which is the break point. Record the volume of potassium chromate standard solution (A) removed. Add 5.00mL ferrous sulfate standard titration rate 4.9) with a straight grid The potassium standard solution (4.3) is tested and the total purple color is reached at the end point. Repeat the above operation until the volume of the potassium chromate standard solution (4.8) consumed reaches a fixed value (H). The volume V of the potassium chromate standard solution consumed is the difference between the A value and the B value. 4.9.3 Calculate the concentration of the standard titration solution using the molar concentration of ferrous iron (NH4)>F(S0,),J, and the sensitivity value is expressed in mol/I. Calculate according to the formula (1>:
CSH,Fe(SU)-S(VV)
-or the sensitivity value of the potassium chromate standard solution, in moles per liter (I/.); V,--the potassium chromate standard solution consumed (1.8, in milliliters (mL) V. —— The volume of potassium chromate (4,9) used for titration, in milliliters (mL) TmI.): — The volume of ammonium iodide standard titration solution (4.9) used for titration, in milliliters (mL). 4.10 Diisocyanate sodium iodide solution (1x/1.). 4.11 Filter cover: GB/T12808A type.
4.12 Titration, GB/T1280A*.
4. 13 Volumetric flask GR/T 12806 A type.
5 Sampling
5.1 Sampling steps
According to GB/T10325 and GB/T17617, 5.2 Sample preparation
According to GB/T5070, 12002, 5.2 Sample preparation 6. Analysis steps
6.1 Number of measurements
Measure under short-term conditions2
6.2 Sample quantity
Weigh the sample according to step 1, and extract to the nearest 0.0001B68
6.3 Sudden test
The pressure of the film should be the pressure factor
13. 1 --30. 00
33. 31 ~b11, 1u
In the female case, short the user:
E.4 Verification test
In the neutral killing condition, the same sample is analyzed and the standard material is integrated. 6.5 Determination
E.5.1 Determination of the sample
6H/T 5C/U.10—2002
E.5.1.1 Put the sample into the end of the end containing 1 agent (4.2), and then mix it with 1 example: 1. Before 1. Disease benefit and use. Lan +8--300r. The temperature is gradually increased to cC1100. Take it out and transfer it to the card plate. The material is evenly attached to the world cold! E.5.1.2 Use a filter to filter the E block and add 20-1.1 boiling sulfur (.7,) mT water at 10°C. Heat the melt until it is clear, wash with water and cover with water, add about 22 ml of nitric acid (1.2>, 1m). Heat the acid (4.3), add 10 ml of concentrated blue water in batches for 10 minutes, add the color of the mixture and cool to air.
6.5.1.4 Add 15 ml of the acid solution (4.6). Add the standard sulfur solution: 1.! No test wave yellow moist head: people, this country road pure stand with flat acid rate density 48 fixed car test record now fixed purple red is the end point. 6.5.2 Blank determination
6.5.2.1 Storage: Mixture (.) Adult sales world exhaustion medium glass cover and process reading chain source: 30 high temperature, send out the steal light culture of the attached cold
6.5.2.2 film method concentrated wipe clean with smoke outside air, effective people have a fee from 2m [. Correction acid (1.7), 5 times burn rod household, hot white pants dead liquid clear Asia, press Erxing pick blue, add water to about m]. 6.5.2.3 Add 5 code silver filter liquid 4.2) 1m1. Please acid and (4.5), heat and add 1r1. Persulfate or ammonium rinse (4.) Keep covering the case red: 5mis~)i. Add chlorinated water to help wave 4, 1. Dye the purple-red color in the bay and take a grid.
6.5.2.4 egg 5,m1. Thin iron connection standard titration velvet reduction 1.5), [3n:1. Thin micro-elastic mixture (,51 and), 3rsl a single quick acid about molten German (4.10>, use 1)m semi-micro tasting wine tube to stand with five front transfer standard guest clear (1.8) standard year test solution baby also: write down the reading of the purple-red.
5.5.2.5 Add 5.0m of the standard dispersion (4.8) and titrate until the color turns red, which is the end point.
6.5.2.6 The product of the reference liquid at the point of concentration (l) is the compensation value (P:. The volume of the reference liquid to be dissolved is V. The total volume of C is C. 7 Calculation of analytical results
chromium oxide mass fraction H x:r:() Counts are expressed in %: Substitution: 2)i 舜;EV 000Vo/1 000x
CBTE07.10—2002
Wuning:
--the volume of the standard solution of ferrous sulfate added to determine the concentration (,), the volume is liter (m) V:--the value of the volume of the potassium ferrous sulfate standard solution (4.8) used for titration, the unit is milliliter (1): W
--the volume of the potassium ferrous sulfate standard solution used for titration, the unit is milliliter (ml/1.); the accurate value of the concentration of the standard solution of ferrous sulfate titration, the unit is [mol/L (mol)/L: the mass value of the material, the unit is gram (g!/SC), the value of the annual pressure, the unit is gram per liter (/m=1M-25. 12): 7.2 The validity of the analysis product shall be determined by the analysis of the new added material under the condition of mutual protection. When the difference between the analysis value of the standard substance and the standard is not greater than the allowable difference, the test analysis value is valid, otherwise it is invalid. 7.3 When the difference between the two valid analysis values obtained in the test does not meet the allowable difference specified in Table 2, the mean of one of the two methods shall be used as the final analysis result. Otherwise, the analysis and numerical processing shall be carried out according to the provisions of Appendix A. 2.4 The new results shall be rounded to the nearest decimal place according to (:H/%170). If the supplier has a reasonable standard, the number of decimal places required for the batch shall be rounded to the required number of places.
8 Allowable difference
The difference between the two independent test results obtained under complex conditions shall not meet the allowable difference listed in Table 1. Table 2
1, 1, n0
5. n1~ 15. x
1a.c1.2o.on
G1~.75, f
#5 #1~·52, 3F
Quality assurance and control
Perform the test in accordance with the provisions of 6.4.
10 Test report
The test report shall at least include the following contents
Commissioning unit:
Name of sample!
Analysis and error:
Difference between the standard (/G20,1-232) and the specified value (if necessary, replace the abnormal phenomenon observed during the test (if necessary, replace the abnormal phenomenon observed during the test) and the test period.
Perform the test in accordance with the provisions of 6.4. bzxZ.net
2,, collect the test report in the form of:
--"Table" as shown in the table.
Certificate
Appendix
(Normative Appendix
Acceptance Analysis Value Procedure
Difference #1.2
GB/I5070,10-200210℃ water:n1. Heat the melt until the liquid is clear, wash with water and cover, add 1 ml nitric acid (1.2>, 1m). Heat the mixture to a thin layer, add 10 ml nitric acid (1.1) and 10 ml nitric acid (4.3) in batches for 13 minutes, add chemical oil (4,5) until the color disappears.
6.5.1.4 Add 15 ml nitric acid (4.6). Add 7 standard sulfuric acid droplets: 1. Do not test the yellow head: the pure acid is 48% pure acid, and the purple-red color is the end point. 6.5.2 Determination of blank
6.5.2.1 Storage: Mixture (.) Adult sales world exhaustion medium and cover with glass and read the chain source: Send to 30 high temperature, send out the stolen light culture attached to the cold
6.5.2.2 Method of concentrated smoke wipe the outside air, effective person filled with 2m[. Corrected acid (1.7), 5 times burnt rod household, hot white pants suddenly drop liquid clear Asia, press Erxing pick blue, add water to about m]. 6.5.2.3 Add 5 code silver filter liquid 4.2) 1m1. Please acid and (4.5), heat and add 1r1. Persulfate or ammonium rinse (4.) Keep covering the case red: 5mis~)i. Add chlorinated water to help wave 4, 1. Dye the purple-red color in the bay and take a grid.
6.5.2.4 egg 5,m1. Thin iron connection standard titration velvet reduction 1.5), [3n:1. Thin micro-elastic mixture (,51 and), 3rsl a single quick acid about molten German (4.10>, use 1)m semi-micro tasting wine tube to stand with five front transfer standard guest clear (1.8) standard year test solution baby also: write down the reading of the purple-red.
5.5.2.5 Add 5.0m of the standard dispersion (4.8) and titrate until the color turns red, which is the end point.
6.5.2.6 The product of the reference liquid at the point of concentration (l) is the compensation value (P:. The volume of the reference liquid to be dissolved is V. The total volume of C is C. 7 Calculation of analytical results
chromium oxide mass fraction H x:r:() Counts are expressed in %: Substitution: 2)i 舜;EV 000Vo/1 000x
CBTE07.10—2002
Wuning:
--the volume of the standard solution of ferrous sulfate added to determine the concentration (,), the volume is liter (m) V:--the value of the volume of the potassium ferrous sulfate standard solution (4.8) used for titration, the unit is milliliter (1): W
--the volume of the potassium ferrous sulfate standard solution used for titration, the unit is milliliter (ml/1.); the accurate value of the concentration of the standard solution of ferrous sulfate titration, the unit is [mol/L (mol)/L: the mass value of the material, the unit is gram (g!/SC), the value of the annual pressure, the unit is gram per liter (/m=1M-25. 12): 7.2 The validity of the analysis product shall be determined by the analysis of the new added material under the condition of mutual protection. When the difference between the analysis value of the standard substance and the standard is not greater than the allowable difference, the test analysis value is valid, otherwise it is invalid. 7.3 When the difference between the two valid analysis values obtained in the test does not meet the allowable difference specified in Table 2, the mean of one of the two methods shall be used as the final analysis result. Otherwise, the analysis and numerical processing shall be carried out according to the provisions of Appendix A. 2.4 The new results shall be rounded to the nearest decimal place according to (:H/%170). If the supplier has a reasonable standard, the number of decimal places required for the batch shall be rounded to the required number of places.
8 Allowable difference
The difference between the two independent test results obtained under complex conditions shall not meet the allowable difference listed in Table 1. Table 2
1, 1, n0
5. n1~ 15. x
1a.c1.2o.on
G1~.75, f
#5 #1~·52, 3F
Quality assurance and control
Perform the test in accordance with the provisions of 6.4.
10 Test report
The test report shall at least include the following contents
Commissioning unit:
Name of sample!
Analysis and error:
Difference between the standard (/G20,1-232) and the specified value (if necessary, replace the abnormal phenomenon observed during the test (if necessary, replace the abnormal phenomenon observed during the test) and the test period.
Perform the test in accordance with the provisions of 6.4.
2,, collect the test report in the form of:
--"Table" as shown in the table.
Certificate
Appendix
(Normative Appendix
Acceptance Analysis Value Procedure
Difference #1.2
GB/I5070,10-200210℃ water:n1. Heat the melt until the liquid is clear, wash with water and cover, add 1 ml nitric acid (1.2>, 1m). Heat the mixture to a thin layer, add 10 ml nitric acid (1.1) and 10 ml nitric acid (4.3) in batches for 13 minutes, add chemical oil (4,5) until the color disappears.
6.5.1.4 Add 15 ml nitric acid (4.6). Add 7 standard sulfuric acid droplets: 1. Do not test the yellow head: the pure acid is 48% pure acid, and the purple-red color is the end point. 6.5.2 Determination of blank
6.5.2.1 Storage: Mixture (.) Adult sales world exhaustion medium and cover with glass and read the chain source: Send to 30 high temperature, send out the stolen light culture attached to the cold
6.5.2.2 Method of concentrated smoke wipe the outside air, effective person filled with 2m[. Corrected acid (1.7), 5 times burnt rod household, hot white pants suddenly drop liquid clear Asia, press Erxing pick blue, add water to about m]. 6.5.2.3 Add 5 code silver filter liquid 4.2) 1m1. Please acid and (4.5), heat and add 1r1. Persulfate or ammonium rinse (4.) Keep covering the case red: 5mis~)i. Add chlorinated water to help wave 4, 1. Dye the purple-red color in the bay and take a grid.
6.5.2.4 egg 5,m1. Thin iron connection standard titration velvet reduction 1.5), [3n:1. Thin micro-elastic mixture (,51 and), 3rsl a single quick acid about molten German (4.10>, use 1)m semi-micro tasting wine tube to stand with five front transfer standard guest clear (1.8) standard year test solution baby also: write down the reading of the purple-red.
5.5.2.5 Add 5.0m of the standard dispersion (4.8) and titrate until the color turns red, which is the end point.
6.5.2.6 The product of the reference liquid at the point of concentration (l) is the compensation value (P:. The volume of the reference liquid to be dissolved is V. The total volume of C is C. 7 Calculation of analytical results
chromium oxide mass fraction H x:r:() Counts are expressed in %: Substitution: 2)i 舜;EV 000Vo/1 000x
CBTE07.10—2002
Wuning:
--the volume of the standard solution of ferrous sulfate added to determine the concentration (,), the volume is liter (m) V:--the value of the volume of the potassium ferrous sulfate standard solution (4.8) used for titration, the unit is milliliter (1): W
--the volume of the potassium ferrous sulfate standard solution used for titration, the unit is milliliter (ml/1.); the accurate value of the concentration of the standard solution of ferrous sulfate titration, the unit is [mol/L (mol)/L: the mass value of the material, the unit is gram (g!/SC), the value of the annual pressure, the unit is gram per liter (/m=1M-25. 12): 7.2 The validity of the analysis product shall be determined by the analysis of the new added material under the condition of mutual protection. When the difference between the analysis value of the standard substance and the standard is not greater than the allowable difference, the test analysis value is valid, otherwise it is invalid. 7.3 When the difference between the two valid analysis values obtained in the test does not meet the allowable difference specified in Table 2, the mean of one of the two methods shall be used as the final analysis result. Otherwise, the analysis and numerical processing shall be carried out according to the provisions of Appendix A. 2.4 The new results shall be rounded to the nearest decimal place according to (:H/%170). If the supplier has a reasonable standard, the number of decimal places required for the batch shall be rounded to the required number of places.
8 Allowable difference
The difference between the two independent test results obtained under complex conditions shall not meet the allowable difference listed in Table 1. Table 2
1, 1, n0
5. n1~ 15. x
1a.c1.2o.on
G1~.75, f
#5 #1~·52, 3F
Quality assurance and control
Perform the test in accordance with the provisions of 6.4.
10 Test report
The test report shall at least include the following contents
Commissioning unit:
Name of sample!
Analysis and error:
Difference between the standard (/G20,1-232) and the specified value (if necessary, replace the abnormal phenomenon observed during the test (if necessary, replace the abnormal phenomenon observed during the test) and the test period.
Perform the test in accordance with the provisions of 6.4.
2,, collect the test report in the form of:
--"Table" as shown in the table.
Certificate
Appendix
(Normative Appendix
Acceptance Analysis Value Procedure
Difference #1.2
GB/I5070,10-2002H/%170 static rate is about decimal places. If the quarterly supply party has the same standard, the number of decimal places required for the batch is rounded off.
8 Allowable error
The difference between the two independent test results obtained under the vehicle complex condition shall not exceed the allowable error listed in the table. Table 2
1, 1, n0
5. n1~ 15. x
1a.c1.2o.on
G1~.75, f
#5 #1~·52, 3F
Quality assurance and control
Perform the inspection test in accordance with the provisions of 6.4.
10 Test report
Let the inspection report at least include the following contents
Commission unit:
Specimen name!
Analysis and error:
Make the standard (/G20,1-232
and the total determination of the difference in the near step (if necessary, the abnormal band phenomenon observed in the test (if necessary: test drive and period.
, x
2,, in the collection
office street release:
--Table" in the Liu points Xu Lan.
Certificate work
Appendix
(Normative Appendix
Acceptance analysis value procedure
of the difference #1.2
GB/I5070,10-2002H/%170 static rate is about decimal places. If the quarterly supply party has the same standard, the number of decimal places required for the batch is rounded off.
8 Allowable error
The difference between the two independent test results obtained under the vehicle complex condition shall not exceed the allowable error listed in the table. Table 2
1, 1, n0
5. n1~ 15. x
1a.c1.2o.on
G1~.75, f
#5 #1~·52, 3F
Quality assurance and control
Perform the inspection test in accordance with the provisions of 6.4.
10 Test report
Let the inspection report at least include the following contents
Commission unit:
Specimen name!
Analysis and error:
Make the standard (/G20,1-232
and the total determination of the difference in the near step (if necessary, the abnormal band phenomenon observed in the test (if necessary: test drive and period.
, x
2,, in the collection
office street release:
--Table" in the Liu points Xu Lan.
Certificate work
Appendix
(Normative Appendix
Acceptance analysis value procedure
of the difference #1.2
GB/I5070,10-2002
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