Some standard content:
UDC:666.658-543.06
National Standard of the People's Republic of China
GB/T 15343—94
Methods for chemical analysis of talcwww.bzxz.net
Promulgated on December 22, 1994
National Mongolian Technical Supervision Bureau
Implementation on August 1, 1995
National Standard of the People's Republic of China
Methods for chemical analysis of talc
Metlmds nr henical ainlyyis oe taleMain content and scope of application
This standard specifies a new method for chemical analysis of talc. This standard applies to the chemical analysis of talc powder in Beijing. 2 Reference standards
GB1341 Appendix
GB 15342 Stone powder
3 General
G8/T15343-94
3. Except for the determination of moisture, the sample should be kept at 1~11gct-2b and placed in a temperature exchanger to cool to room temperature before weighing. 3.2 Unless otherwise specified, the test should be accurate to 0.1. The constant weight referred to in the formula refers to the total weight of 0.3mg
3.3 The water referred to in this method refers to the water solution without high temperature after being desorbed or treated by other methods. The water used is an aqueous solution unless otherwise specified.
3.4 The final concentration of the contact liquid is the concentration of the liquid at 1T/1.), if (11) < 1 + 2, (+) refers to the ratio of the volume of the liquid to the volume of the liquid.
3.5 The reagents used in the new test should be analytically pure or high-grade pure reagents: the reagents used should be standard reagents unless otherwise specified. The water used should be standard or grade nitrogen water if not specified. 3.6 Except for the measurement of the lost area, the other measurements should be carried out with a blank test and the results should be corrected. 3.7 Unless otherwise specified, the numerical value of the new result (%) should be rounded to the nearest decimal place. 4 Samples
4.1 Detailed sampling of the test
4.1.! Slide sample collection shall be carried out in accordance with GB15341.4 1.2 Condensation sample collection shall be carried out in accordance with 1 or 4.2 Sample holding basket shall be carried out in accordance with GB1341. GB15312. The sample sent to the laboratory shall not be less than 1 kg (passing 180m sieve). It shall be reduced by quartering or staggering. 192. Grind until the sample passes through 75m sieve, and the end life does not exceed 50%. Then use quartering or staggering to reduce 25%. Finally, grind until all of the sample passes through 75m sieve. Use a magnet to remove the liquid that enters when the sample is crushed. Stir well and set aside. 5 Analysis method 5. [Determination of appearance] National Thermal Technology Supervision Week 1994-12-22 Approved 1995-08-01 # 5.1.1 Method summary GB/T 1534394
Let the desired condensation, magnetite, organic matter and other volatile substances be decomposed by commercial lamp, and then the quality difference is calculated and recorded after burning. 5.1.2 Analysis
Weigh the sample accurately to 0.00U1 or the end of the porcelain step that has been constant, and place it on the ground at an angle. Put it into a high temperature protection room, take it out and cool it to room temperature, and keep it at 100℃, and burn it until it reaches room temperature. 5.13 The percentage of salt loss (X is calculated by formula: -×100
5: The data before calcination and the pressure base of the sample-8
The quality of the non-calcined sample after calcination and the test state: the amount of the sample. 5.1.4 The allowable difference of the parallel research results is shown in Table 1. Loss of salt·salt loss ... 00
Allowable error, %
If the results of the parallel determinations are within the range of use, the technical average value is the fixed result, the special rule should be determined again. 5.2 Determination of silicon dioxide
5.2. Animal coagulation method-filtration saturated blue colorimetric method (A method) 5-2.7.1 is the method proposal
The silica is melted with sodium carbonate and restored with animal glue solution in hydrochloric acid medium. After heating, burning and hydrogen ammonia treatment, silicon is released in the form of tetrahydrofuran. After that, the residual silicon dioxide in the filtrate is quickly determined by blue colorimetric method. 5.2.1.2 Reagents and apparatus
Anhydrous sodium nitrate
salt (1-1,2+98
silver nitrate Get the concentration (100/1.), etc.] * Silver nitrate is dissolved in 50[. water, add 1 drop of nitric acid (1+1, dilute with water to 100mL;
Animal glue drop liquid (10/: Put 1 sieve of white stock in L water of about 7C (prepared with) oxygen
Vegetable acid (1+1): Slowly add 1 volume of sulfuric acid to a large volume of water and mix: Phosphoric acid (1+4) +
Perchloric acid is used for dissolution (1008/L): Weigh 10g of perchloric acid in a material cup, add a certain amount of water to dissolve and dilute to 100mL; Acid solution (56/): Weigh 5e of acid in a plastic cup, dissolve in four times of water and dilute with water to 10mL: Potassium pyrophosphate +
Anti-blood filtration (50 = Area/L), time taken: Silica standard solution (A) (1mL solution contains 0.2g silicon dichloride): Accurately weigh 0.10Ug of silicon dioxide that has been burned at 000C for 1h (full standard or spectrally pure reagent) and add it to the solution. * Anhydrous acid spray, mix well: Cover with 1B anhydrous sodium carbonate, melt at high temperature for 5~10m, cool and remove the molten block from a beaker containing about 300mL hot water with hot water, add 2
CB/T15343-94
New dense solution, cool to room temperature, transfer to a 500mL container, bring to standard with water, mix, and then transfer to the following plastic bottle for storage: 2. Silica standard solution (B) (1mL solution contains 0.02mg silica bomb). Accurately pipette 10.00mL silica standard solution (A) into 100㎡ container bottle and dilute with water to standard. Mix (prepare when using). Warm water bath,
y: 5.2-1.3T fried curve drawing
Accurately take 0.00, 1.00, 2.00, 3.00, 4.00, 5.00.6.00mL = silica standard solution (Z5, put into 1Hml container bottle, add water to about 30)ml, add (5m hydrochloric acid 1+1) add 5mL ascorbic acid according to the drop minus 60g/1.), mix, according to the room temperature at different times, then add 5L of clotting acid (1+!) filter spoon, add ml. ascorbic acid solution 5/), mix with a spoon, mark the water tax sample, and mix. This series of standards contains 1 microliter of silicon dioxide (0.00, 0.02, 0.04, 0.06, 0.08, 0.10, 0.12mB). After being irradiated to 10211nm, the photometric value is determined on a spectrophotometer at a wavelength of 530nm using a 10mm colorimetric solution and water as a reference. Then, the working curve is prepared with the measured photometric value as the ordinate and the irradiation of the colorimetric solution as the coordinate. Table 2
Xuan, t:
an~·35
5.2.1.4 Analysis Steps
Minimum time, min
Take about 0.5g (accurate to 0.0001) of sample in platinum, add 3g of anhydrous sodium ferrate, mix well, add 1g of anhydrous sodium carbonate, mix well. Place in a high temperature furnace or on a blowtorch> heat to 950~1000V, melt for 30min, take out, and transfer to glass The melt is evenly attached to the inside of the ground, and then cooled. Use hot water to take the molten block into a 150-25mm wide evaporating bath, add 40ml of hot acid (11) to the surface, and slowly add 40ml of hot acid (11) to the evaporating bath. After the reaction stops, take the bottom layer and add the acid (1+1) to cover it. Combine the washing liquid with the evaporating bath, rinse the surface layer and the edge of the evaporating bath with water, and immediately evaporate it in a boiling water bath to heat the latent liquid to a wet state, and then press the evaporator. Add 20ml of hot acid (11) to the evaporating bath. Mix well and stir, keep warm in 70~80℃ for 5min, add 10ml animal gelatin solution (10g/L), stir well and keep warm for 10~15min, remove, add 30ml hot water, stir to dissolve the heat, cool, filter with neutralized paper, wash with warm hydrochloric acid (2+93) and swirl 6~8 times, collect the filtrate and washing liquid in a 300mL beaker. Clean the blood with a small piece of paper. , wash with warm water until the precipitate is slightly depleted of light, and then test with a 1/2 ml solution. Put the precipitate together with the filter paper into a platinum solution, dry it, and calcine it at 1000°C for 1 hour. Take it out, cool it to room temperature in a 10-well reactor, weigh it, and calcine it repeatedly until it reaches a constant weight. Moisten the precipitate with a small amount of water, add 2 to 3 ml of sulfuric acid (1+1), 5 to 8 ml of hydrochloric acid, heat it until it is almost 1/2, remove the precipitate and cool it, and then add 31 ml.Hydrogenated acid, heat until sulfur trioxide is completely white, burn at 1000℃ for 10~15min, remove, cool to room temperature in a desiccator, weigh. Repeat burning until the temperature is constant. Melt potassium pyrophosphate with 5% pyrophosphate. Cool, dissolve the molten material in hot water and combine in a beaker.
To destroy animal glue, add 1% nitric acid and stir for 30min until the smell of oxide disappears. After cooling the solution to room temperature, transfer it to a 250ml bottle, dilute it with water, and measure the amount. This is the sample solution (A), which can be used to determine the content of silicon dioxide, calcium, and silicon dioxide left in the solution.
Take 10.00 ml of the experimental filter (A) and put it in a 100 ml beaker. Add 50 g/L sodium bicarbonate (100 g/L) and a small amount of sodium bicarbonate. Heat to boiling and keep for 2 min (do not evaporate to dryness). Remove and cool slightly. Rinse the surface with water. Weigh the filter into a 100 ml volumetric flask and add water to about 5 g. The following steps are the same as those for drawing the working curve. 5.2.1.5 Calculation of results
The content of silicon dioxide in 109ml of the sample is mg! The ratio of the total volume of the test sample to the volume of the sample is: The amount of the sample is
5-2. 1. 6. Tolerances
Parallel measurement results are allowed to be within the allowable range. The results are given in Table 3.
One-core extraction point, the difference
The difference
The result of parallel determination is within the allowable range. The polysilicon dioxide content is determined by the technical level and the bias. Formula, latest determination, 5.2.2 Polysilicon dioxide concentration method 1
5.2.2.1, method summary
Filter phase colorimetric method (B method)
The test column is melted with sodium hydroxide, and precipitated in hydrochloric acid medium without ethane to precipitate silica, and then treated with indigo plant, ashing, calcination, or chlorination, and then in the form of tetrahydrofuran. The residual silica in the filtrate is determined by platinum blue colorimetric method 5.2.2.2 Reagents and instruments
Sodium bicarbonate anhydrous:
Acid:
Hydrochloric acid (1-1,2+98)
Ethylene oxide solution (2.5g/L): weigh 0.25g of ethylene oxide in a beaker, add 100mL of water, bubble for a while: stir and dissolve: can be ~3% sodium bicarbonate (1+2). Store in a plastic bottle; e.
Hydrogen iodide;
Hydrogen iodide (1+1.1+4)
Sodium bicarbonate (50g/1.)
Ascorbic acid (50:1)
Trioxide standard filter, the preparation method is the same as Standard 5.2.1.2: Water chestnut;
k. Spectrophotometer.
5.2.2.3T. Preparation of the composition
same as the standard No. 2.1.3.
5.2.2.4 Analysis of the unsatisfactory step
Weigh 0.5g of the sample accurately to 0.001, add sodium ferromagnetic acid, standard, and then take 1% anhydrous carbon. Place it in a high-temperature annealing furnace (reduced by the burner), gradually turn off the temperature to 0.501000℃ and keep it for 2U~90min, and finally turn it over to the address of Wa, so that the molten material is evenly attached to the ground, and the molten block is cooled and collected in 150~25ml of hot water. Evaporation blood , cover the surface of the filter, add 40mL of solution (111) slowly from the mouth. After the reaction stops, collect the surface of the filter, and use hydrochloric acid (1+1) to clean the end. The washing liquid will be added to the honey evaporated solution, and the surface of the solution and the curling part will be washed with water. Put the evaporated solution on a bullet water bath, heat the evaporated silica gel to precipitate completely (volume about 1IrrtL), add 15mL of the filter paper, stir under 5mL of 2.5g/L of ethane), let it stand for 5min+, then filter it at medium speed, wash the precipitate with hot salt formaldehyde (2+8>) for 8 to 10 times, and then wash it with hot water until there are no more ions (use silver nitrate to control the test), and add the thinner and washing liquid to a 250mL container.
The precipitate is put into the world together with the natural paper, dried, ashed, calcined at 1000℃ for 1h, taken out, and placed in a desiccator until it reaches home, and weighed. Burn again until the precipitate is heavy.
GB/T15343-94
Moisten the precipitate with a little water, add 2~3 ml of 1+1,5~8 ml of chlorinated acid. Add 3 mL of argon and heat until almost dry, cool slightly and then add 3 mL of argon, evaporate until the 3% chlorine is completely removed, burn at 1°C for 10~12 min, place in a refrigerator and cool to room temperature, then burn again until the precipitate is stable. Melt the residue with 0.5% potassium sulfate and cool with hot water. Then filter the mixture and cool. Dilute with water and mix thoroughly. Take the above solution and put it into a bottle with a certain volume. Draw the line again according to the same operation steps. 5.2.2.5 Results and calculation
Time This standard 5.7. 1. 5.
5.2-3 Silicone removal (core method)
5.2.3.1 Summary of the method
In the presence of excessive radiation, potassium ions are present in a strong acidic solution to form potassium silicate (K,SiF>). After precipitating, washing and neutralizing the precipitate with the residual acid on the filter paper, water is added to hydrolyze the precipitate to generate a certain amount of hydroxyl. After that, the precipitate is titrated retrogradely with a single chemical identification standard solution using tantalum as an indicator.
5.2.3.2 Reagents
Sodium hydroxide: Granular:
h. Nitric acid F
d. Hydrochloric acid + 57
Potassium hydroxide is ground and stored for later use:||tt ||[. Fluoride solution (150B/L): Put 15g potassium fluoride (KF-2H,O) in a plastic cup, add 50mL aqueous solution, add 20mL nitrate, and mix with water to 100mL: Add 20mL nitrate solution under stirring until the mixture is mixed for 3 minutes, and read the potassium hydroxide solution (50g/) in the mixing bottle with a quick filter paper:
b. Potassium oxide-ethanol solution (50/L) 5 potassium oxide is dissolved in 50mL water, cut into 5Cml.95% ethanol, mix: 1. Phenol indicator solution (1/L); dissolve 1 ketoacetate in 10ImL95% ethanol, adjust to neutral with sodium hydroxide solution + sodium hydroxide standard solution (Na2O3 = 0. 1mn)/) Add 60% sodium hydroxide to 10% water, mix thoroughly and store in a sealed barrel (with a sodium lime drying tube) or a hard glass bottle. For calibration, weigh about 0.8g (accurate to 0.0001g) of potassium dipotassium benzoate in a 400mL beaker, add about 150ml of freshly washed cold water (the cold water is neutralized with some sodium oxide standard until the acid is slightly reddish), and dissolve it. Then add 6 to 7 drops of phenolic acid indicator and titrate with ammonia oxide auxiliary standard until the acid is slightly reddish. The molar density (c) of the sodium hydroxide standard solution is calculated according to formula (3): C
mX1000
The molar density (c) of the sodium hydroxide standard solution to silicon trioxide The flux density (Ta%0,> is calculated according to the formula (4>, and its value can be approximately expressed as a decimal: Tso.
Wherein: the volume of potassium dipotassium hydroxide -R
204.21——the volume of sodium hydrogen monoxide standard solution consumed when these drops of potassium dipotassium hydroxide are dissolved.mL; 15.02——1/4=the volume of silicon dioxide in 1
Tso,1ml. The amount of sodium hydroxide standard solution equivalent to Tso.mg5.2.3.3 Analysis steps
Weigh about 0.5g (accurate to 0.00012) of the sample, add a few drops of anhydrous ethanol, 8 drops of hydrogen monoxide. Cover with a lid (dissolved 5
GB/T 15343—94
There is a large air removal), put it into a high-temperature furnace. Start at low temperature at 700~5 for 1h (take out the solution several times in the middle), finally cool it into a beaker containing 15DmL hot water, wait for the solution to be completely dissolved, collect the solution and rinse it with hot water. Under stirring, add 30mL hydrochloric acid and 1mL nitric acid at a time. Wash the snail and cover with a gap (1+5>) and put them in a beaker. Heat the beaker to a microfiltration level and keep it for 5~10min. Remove it and cool it to room temperature. Adjust it to 25mml. Put it in a bottle, mix it with water, and change the sample to (1). Ensure that the liquid is provided with silicon, iron, aluminum, silver, calcium, and other elements. Take 3.00ml of the test solution (B) in a 200mL plastic beaker, Add 10-15mL of sample, add 11% of chemical solution (150/10) to cold water, stir, add potassium hydroxide, cool in cold water and place for 21m!m, pass through filter paper at medium speed, mix the sample and precipitate 3 times with 8% of chemical solution, put the precipitate together with the filter paper into the original plastic cup, add 1% chlorinated ethanol solution (1/L) and 1% phenol indicator (1CR/1), filter with 15ml/1.2. For any remaining acid in the cup: carefully change the paper towel and wipe the cup palm, keep holding the cup until the red color disappears, then add 200ml of water (the standard sodium hydroxide solution has been freed, i.e., monophenol red). Add 0.15a0.1% sodium hydroxide standard solution to the cup until it turns slightly red: 5.2.3.4 Calculation of results
-. The percentage of silica gel (X) is calculated according to formula (5): I × VXr
X10
Wherein: Tar,
-1ml of standard sodium hydroxide solution is equivalent to the mass of silicon dioxide, mg is the volume of standard sodium hydroxide solution, mL is the ratio of the total volume of the sample to the volume of the sample solution; the volume of the sample is 8.
5.2.3.5 Allowable difference
Same as 5.2.1.6 of this standard,
5.3 Determination of trivalent iron and phthalocyanine colorimetric method
5.31 Phthalochromic colorimetric method (Method A)
5.3.1.1 Summary of method
Ascorbic acid is used to reduce trivalent iron to monovalent iron. When pH>2., monovalent iron and phthalocyanine can form a red complex, and its photometry is measured at 510°C using a spectrophotometer.
5.3.1.2 Reagents and instruments
Ammonium chloride (1+1);
Hydrochloric acid (1+1>,
p-nitrophenol indicator (508/L);
Hydrochloric acid (50g/L:
O-phenanthroline solution (/ Dissolve 0.1g o-phenanthroline in 1m ethyl acetate, add 9ml boiling tartaric acid solution (
|g, standard ferric oxide (1ml solution contains 0.05mg ferric oxide): weigh 0.100g ferric oxide (the high-boiled reagent is pre-calcined at 950~1000℃) in a 300mL beaker, add 50ml water, 30mL hydrochloric acid (1+1), 2ml ethanol, heat at low temperature until the solution is completely dissolved, cool to room temperature, and simmer in a 2000mL bottle. , dilute to the mark with water, insert spectrophotometer.
5.3.1.3 Drawing of working circle
Take 0.00, 1.00, 3.00.5.00.7.00mL of three kinds of standard solution of dihydrogen dioxide (containing 0, 00, 0.05, 0.15, 0.25, 0.35mg dihydrogen dioxide respectively), put them into 100mL medium, dilute with water to about 50mL, add 4mL of 100g/L filter, 1~2 drops of p-nitrofuran indicator (5g/L), add ammonium hydroxide solution (1+1) drop by drop until it turns yellow, then add hydrochloric acid (1+1) until it turns from yellow to colorless, add 4mL of 1% hydroxylamine solution (50R/L), 10mL of o-phenanthroline solution (1g/L) and add water 6
CB/T 15343—94
Dissolve to the mark, mix, add 20mm, and use a 10mm colorimetric filter to measure the absorbance of the solution at a wavelength of 68 nm. Then, use the measured absorbance as the ordinate and the concentration of the colorimetric solution as the ordinate to draw a working curve. 5.3.1.4 Analysis Steps
Take 10.00 μl of the sample prepared according to the technical standard 5.2.1.4 (A) or the sample prepared according to 5.2 and 3.3 of this standard (B>) in a 100mL volume, add water to about 30mL. The following steps are the same as those for the preparation of the line. 5.3.1.5 Calculation of Results
The percentage of the chemical disulfide contained () is calculated according to (6): CXR
m×100g×100| |tt||In the formula, e is the content of dinitrogen in mg in 100 mL of the colorimetric solution obtained from the working curve; the ratio of the total volume of the sample dissolved to the volume of the sample dissolved! The quality of the sample,
5.3.1.6 Permissible error table 4 for parallel determination results.
The content of dinitrogen is
Permissible error %
If the difference between the two determination results is within the permissible range, take the arithmetic mean as the determination result, otherwise a new determination should be made. 5.3.2 EDTA complex determination method (B method)
5.32.1 Summary
In the solution at pH 1.8~-2. C and 6L-~?0C, use sulfonic acid chain as indicator and use ETA standard elution range for determination. 5.3.2.2 Test
ammonium hydroxide solution [1+1);
acetic acid (1+1)
sulfonic acid water granules indicator solution (1 called R/): fine test paper·PHO.5~5.0
calcium chlorophyll methyl ... 1g potassium hydroxide is dissolved in water and diluted to 100ml. It is stored in a plastic bottle. Carbon aldehyde transfer standard solution is reduced. Take 0.g (accurate to 0.0001g) calcium phosphate (high purity reagent) that has been dried at 105~110℃ for 2h and put it in a 40ml beaker. Add about 100ml water. Cover the surface with salt (100ml) along the mouth of the cup until the carbon cavity is completely dissolved. Heat for 3-5min. Remove and cool to room temperature, transfer to a 250mL container, dilute with water to the standard, according to Z diaminetetraacetic acid disodium (abbreviated as EDTA) standard solution box [e(ELYIA) = C,015 mol/L: Weigh 56 g EDTA in a 100 ml beaker, add 6 mL water, heat to dissolve, cool, filter, and add water to 100 mL. Calibration method: Accurately take 25.00 mL of calcium carbonate standard solution in 400 ml of water, dilute with water to about 200 nl, add appropriate amount of CMP source indicator, add potassium hydroxide (200 g/L) dropwise under stirring until green fluorescence appears, then add 1-2 mL of EDTA standard solution to clarify until the green fluorescence disappears and turns red. The full range of FTTA standard solution for calcium carbonate, iron trioxide, aluminum trioxide, calcium oxide, and pyrolysis is calculated according to formula (7) to formula (11), and its value is rounded to four decimal places. In the formula: Tco, GB/T 15343-94 Means, X 5. 797 7
CxYsx0.5603
CXV0.4028
1.NUTILEIITA standard solution is equivalent to the mass of carbonated urea, mB!-1.00ml.EDTA standard solution is equivalent to trioxide: soft drug base, m1.n(L.FTTA standard solution is equivalent to the mass of dioxide from low.rngTL--.1.(0mLELTA standard solution is equivalent to the mass of calcium oxide method mR:Tma|| tt||1.C0mLEITA standard solution is equivalent to the mass of magnesium oxide, mg: 1.(C0mmL) calcium carbonate standard solution contains the mass of calcium hydrate, mg: the product of calcium carbonate standard solution, m
the volume of EDTA standard solution consumed during calibration, mL; the molecular weight of ferric oxide;
the molecular weight of aluminum oxide,
the molecular weight of calcium carbonate:
the molecular weight of calcium carbonate.
5.3.2.3 Analytical step
Accurately divide into 50.00mL of the standard solution 5.2.1.4 Prepare the test solution (A) or the original solution 5.8.5.9 Prepare the sample solution (B) in a 300mL hot cup, dilute with water to about 100mL, and adjust the pH of the solution to 1.8-2.0 with ammonium hydroxide (1+1). (Use precision PF test paper, add a small amount to 70 C, add 10 drops of sodium EDTA (100/1) and EDTA (c(EDTA) = 0.01mnl/1. Slowly cool to a fading color (pure color when the iron content is low). The temperature should not be lower than 6C. 5-3.2.4 Calculation of results
The percentage of ferric oxide (X,) is calculated according to formula (12): x.
T×V×A
m X 1 H
Where: T, — 1. ml. EDTA standard rate equivalent to T trioxide, rg 1V——volume of EDTA standard consumed during titration. mL+ and — — ratio of total volume of test solution to volume of sample solution; — mass fraction of sample.
5.3.2.5 Allowable error
The allowable error of parallel determination results is shown in Table 5.
Fe2O3 content.GB/T 15343 94:1-1. If the results of the determination are within the allowable range, take the arithmetic mean as the test result. If necessary, repeat the test. Determination of reduced dichloromethane 5.4.1 Back titration method (A) 5.4.1.1 Method 1. Add aluminum-titanium-based EIA standard solution to the titration solution, pH 3.64.C. Use PAN as the indicator. Use copper sulfate as the standard back titration solution to make ETA 5.4.1.2 Test solution: ammonium hydroxide solution b. acetic acid-sodium ethyl acetate buffer Dissolve (p.3>, 2. Sodium acetate in water. Add 8umL glacial acetic acid, then dilute to 1000mL with water, score;
c. 1-2-pyridine)-2-pyridine (abbreviated as PAN) refers to water; 1.2PAN is dissolved in 1001mL of ethyl acetate:
d. Flow acid to standard melting point (CuSO,>=0.015mal/.), sample 3.7g flow to makeStandard solution c(EITA)=.015mDl preparation and calibration method is called standard 5.3.2.2
f. Determination of the volume ratio of EDTA standard solution to sulfuric acid standard filtrate: 1U.1~15.SmC.015mal/LEL>1A standard solution is placed in a 400mL beaker and diluted with water to 235ml..11jml. of acid-acetic acid buffer solution (H4.3, add salt and bring to a boil, remove, cool slightly, add 4~5 drops of PAV indicator solution, and titrate until bright purple. The volume ratio of EDTA standard solution to sulfuric acid standard filtrate (K> formula <13) is calculated as: W
In the formula, K: 1.CGmL. For acid standard filtrate, F) Volume of TA standard solution, mL: Volume of EDTA standard solution, L
V, - the volume of EDTA standard solution, m, 5.4.1.3 Analysis steps
tAccording to the standard 5.3.2.3, after the standard solution is fully recovered, accurately add 10.00~20.00ml. 0.015mol/L EDTA standard solution, then dilute with water to about 2cm), add the solution to 7U~80. Adjust the pH value to 3.5~4.0 with oxygen oxidizing solution (1+1). Add 15mL acetic acid-catechol diacetate (pH 4.3), boil for 2~3min, remove and cool slightly, add 4~5 drops of PALV indicator solution, filter and mark with copper thiocyanate to obtain a semi-bright purple color. 5-4.1.4 Result: The percentage of calcium oxide (X) is calculated according to formula (14): Taa × (V, -V,) × n
× 1-0.64X
.. (14)
Wuzhong: Ta
GB/T 15343
1.niT.FNTA standard minus the mass of dilute trioxide.n1g volume of DTA standard solution, mL:
The volume of the titrated sulfuric acid standard solution, mL1.00nuI.The concentration of sulfuric acid standard solution is equivalent to the volume of the EETA standard filtration product.mL.1The ratio of the total concentration of the sample to the total concentration of the sample.B:
Minus the conversion factor of aluminum oxide.
According to this standard, the percentage of titanium dioxide obtained by 5 pools is 5.2.1.5. The allowable difference is taken as the result of the determination.
The content of titanium dioxide is allowed to be determined by parallel filtration. If the difference between the results of parallel filtration is within the allowable range, the arithmetic mean is taken as the determination result. Two periods, should be re-determined, 5.4.2 Total benefit chemical subtraction method (B) method
5.4.2.1 Small method to extract
Are all added to the titanium. Phase. The EDTA standard potential reduction. Adjust pF=1, cook Buddha, with salt solution and drop EDTA, to measure the total iron, lead, and then the soft and number content measured by the ratio method (converted into tantalum trioxide), which is the content of aluminum dioxide, 5.4.2.2 Reagents
nThis standard i.4.1.2
5.4.2.3 Summary steps
Accurately take 50.00mL of the sample solution prepared according to the standard 5.2.1.4(1 ml contains 0.1 mg titanium monoxide): Accurately weigh 0.1000% titanium oxide (high purity test material or optical microscope), calcine at 950℃ for 10min in a flask, add 2R pyrosulfuric acid, melt on a blowtorch at high temperature until suitable, cool, bleed with sulfuric acid (1 + 9), and heat to 50-60℃. After the molten block is completely dissolved, cool to room temperature. Transfer to a 1000mL mother bottle, add sludge (1 + $) to bring the sample to standard, and mix with: titanium oxide standard solution (Z >(1mL of drop micro contains 0.<1zmg of titanium dioxide) Take 1Cml of titanium dioxide standard drop liquid (A), adult 500ml volumetric bottle, use grinding medium (1-9) to push to the mark, mix with spoon: f. Spectrophotometer.
5.5.1.31. Drawing of composition
Respectively, put 0.00, 1.00+3.00, 5.00, 7.00, 9.00mL of titanium dioxide standard drop liquid (B) (containing 0.00, 0.02 .0.06.0.10.0.14,0.1 mg titanium dioxide), add 10 mL hydrochloric acid (1+2), 10 mL ascorbic acid, 5 mL 55% ethanol, 20 mL diamine methane, and then use water as the scale line and mix well. After 40 minutes of silk, use a spectrophotometer to make 10 mL colorimetric blood, use water as the ratio: measure the absorbance of the solution at 2 ° C m of the filter. After silk, take the measured absorbance as the number, and the relative humidity as the standard, and draw the working curve: 5.5.1 .4 Operation steps
Accurately collect 25.00 ml of the sample solution (A) prepared in 5.2.1.4 of this standard or the sample solution (B) prepared in 5.2.3.3 of this standard and put it into a 100 ml container. Add 10 ml of hydrochloric acid (12) and 10 ml of ascorbic acid. Place 5 L of 20 ml of diammonium chloride solution on top. The following operation steps are similar to those in the previous operation. 5.5.1.5 Calculation
The percentage of iron in the two bottles (X) is calculated according to formula (16). =
1000100
Wherein, the content of hydrogen monoxide in 100mL of the sample obtained from the working curve, mg! The ratio of the total volume of the sample solution to the volume of the sample solution taken out of the test tube, g.
5.5.1.6 Allowable difference
The allowable difference of parallel titration results is shown in the table. Table?
Fe(III) content, %
.D. 50
Allow some,
If the difference between the parallel determination results is within the allowable range, take the arithmetic mean as the determination result. Otherwise, the determination should be repeated. 5.5.2 Hydrogen peroxide colorimetric method (B method)
5.5.2.1 Method summary
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