Some standard content:
National Standard of the People's Republic of China
Analytical method of the chemical composition in the quartz glass
1 Subject content and scope of application
GB/T 3284--93
Replaces GB328482
This standard specifies the reagents, materials and instruments used in the chemical composition analysis of quartz glass, the preparation and decomposition of samples, the analysis steps and the method of expressing the results.
This standard is applicable to the chemical composition analysis of quartz glass, high-purity quartz glass and its raw materials, crystal and silica. 2 Analytical methods
2.1 Chemical analysis method
2.1.1 Determination of loss on ignition and silicon dioxide
2.1.1.1 Summary and principle of the method
The sample is decomposed by sulfuric acid and hydrofluoric acid to convert all silicon dioxide into silicon tetrafluoride and remove it. The reaction equation is as follows: SiO, + 6HF→H2SiF + 2H,O
H,SiF→SiF,++ 2HF+
2.1.1.2 Reagents and instruments
Hydrofluoric acid (HF)2: high-grade pure.
Sulfuric acid solution: 1+4, high-grade pure.
Hydrochloric acid solution: 1+1.
High-purity water: secondary exchange water.
High-temperature furnace.
Platinum crucible.
2.1.1.3 Samples
2.1.1.3.1 Laboratory samples
The samples for inspection shall not be contaminated and shall have a mass of not less than 20g. 2.1.1.3.2 Samples
After breaking the laboratory samples into pieces or quenching the raw materials with water, take a certain amount of pieces (particle size <5mm) and cover them in hydrochloric acid solution and boil for about 10 minutes, then wash them thoroughly with high-purity water, dry them, and grind them into fine particles with an agate mortar to a particle size of about 0.125μm (120 mesh), and store them in a sample bottle for later use.
2.1.1.4 Analysis steps
2.1.1.4.1 Test sample
Weigh two portions of the test sample of about 1g which has been dried at 110°C for not less than 2h, accurate to 0.0001g, and place them respectively in two platinum crucibles which have been calcined to constant weight at 950-1000°C.
2.1.1.4.2 Vacuum test
GB/T 3284—93
Except for not adding test sample, adopt the same analysis steps, reagents and dosages as those for the determination and carry out parallel operation. 2.1.1.4.3 Determination of loss on ignition
Place the platinum with the sample in a high-temperature furnace at 950-1000°C and burn for no less than 1 hour, then transfer it to a desiccator and cool it to room temperature before weighing it. Burn it for another 20 minutes. Cool it and weigh it. Repeat the burning until the weight is constant. Keep the constant-weight sample A for the determination in 2.1.1.4.4. 2.1.1.4.4 Determination of silicon dioxide
Add a few drops of high-purity water to the constant-weight sample A obtained in 2.1.1.4.3 to moisten it. Then add 5 drops of sulfuric acid solution and 5ml. hydrofluoric acid, evaporate it on an electric furnace at 80-100°C until it is nearly dry, remove the crucible, cool it down, wash the crucible wall with a small amount of high-purity water, then add 3mL of hydrofluoric acid, evaporate it on a low-temperature electric furnace until it is nearly dry, and wash the crucible wall with a small amount of high-purity water. After evaporating it again, increase the temperature to drive out all the sulfur dioxide. After cooling, wipe the outer wall of the crucible with wet filter paper, and burn it at a high temperature of 950~1000℃ for 30min. Move it into a desiccator and cool it to room temperature, then weigh it and burn it repeatedly until the weight is constant.
2.1.1.5 Expression of analysis results
2.1.1.5.1 Loss on ignition
Loss on ignition is expressed as the mass percentage of high-temperature ignition loss, calculated according to formula (1): X= m=m2 × 100
Where: X-—Loss on ignition of the sample, %;
m--Sample mass basis.g;
ml-—Mass of the crucible and sample before ignition, g; m2—Mass of the crucible and sample after ignition·g. The result should be expressed to two decimal places.
2.1.1.5.2 Silicon dioxide content
The content of silicon dioxide is expressed in mass percentage and calculated according to formula (2): Xx =m=m+m× 100
Wherein; X, — silicon dioxide content in the sample, %; m — mass of sample·g;
m, — mass of crucible and sample after calcination, g; mz-mass of crucible and residue after hydrofluoric acid treatment, g; m, mass of residue in blank test, g.
The result should be expressed to two decimal places.
2.1.1.6 Tolerance
The tolerance of the analysis result of silicon dioxide content is within 0.1%. 2.1.2 Determination of titanium dioxide in low expansion quartz glass 2.1.2.1 Summary of method
The sample is decomposed by sulfuric acid and hydrofluoric acid, and then determined by disodium ethylenediaminetetraacetic acid (EDTA) complexometric titration. 2.1.2.2 Reagents
2.1.2.2.1 Hexamethylenetetramine.
2.1.2.2.2 Hydrofluoric acid: high purity, 40% (V/V). 2.1.2.2.3 Ammonium hydroxide: 1+1.
2.1.2.2.4 Sulfuric acid solution: 1+1.
2.1.2.2.5 Hydrochloric acid solution: 1+1.
(1)
2.1.2.2.6 Zinc acetate solution: 0.01mol/L. GB/T 3284-- 93
Weigh 1.6g zinc acetate, accurate to 0.1g, and dissolve it in a small amount of water. Adjust the pH to 6 with acetic acid. Dilute to 1000ml with water. 2.1.2.2.7 Calcium oxide standard solution (1mg/ml): Weigh 1.7848g of calcium carbonate (superior purity) dried at 105C for not less than 1h, accurate to 0.0001g, in a 200ml beaker, add a small amount of high-purity water, drop hydrochloric acid solution to dissolve, heat and boil for 5min, cool. Transfer to a 1000ml volumetric flask, dilute to scale with high-purity water, and shake well.
2.1.2.2.8 Hemi-monocresol orange indicator solution: 5g/1. Weigh 0.5g of hemi-xylenol orange indicator, accurate to 0.1g, and dissolve in 100ml of water. 2.1.2.2.9 EDTA standard titration solution, 0.015mol/L. a. Preparation method
Weigh 5.5g of EDTA, accurate to 0.1g, dissolve in a small amount of water, and dilute to 1000ml with water b. Calibration method
Put 15.0ml of 1mg/ml calcium oxide standard solution in a 300ml beaker, dilute with water to about 150ml, add 20% sodium hydroxide solution until the solution pH is about 12. Add 2ml of calcium indicator (the ratio of calcium indicator to dried sodium chloride is 1+50, grind and mix well). Titrate with 0.015mol/1 EDTA standard solution until the solution changes from purple-red to pure blue. The concentration of EDTA standard titration solution is calculated according to formula (3):
56.08 x V
Wherein: C--EDTA standard titration solution concentration, mol/L; calcium oxide basis, mg;
V--volume of EDTA standard titration solution consumed during titration, mL; (3)
56.08--the mass of calcium oxide in grams equivalent to 1.00mL EDTA standard titration solution Lc (CaO) 1.000mol/1). C. Volume ratio of zinc acetate solution to EDTA standard solution Take 10.0ml of EDTA standard titration solution in a 300mL beaker, dilute with water to about 150ml, add 1g of hexamethylenetetramine and 3-4 drops of hemi-xylenol orange indicator, add hydrochloric acid solution until the solution turns yellow, and add zinc acetate solution until the solution changes from yellow to orange-red. The volume ratio is calculated according to formula (4):
Wherein: u-——the volume of EDTA standard titration solution equivalent to each milliliter of zinc acetate solution; V——the volume of zinc acetate consumed during titration, ml. 2.1.2.2.10 platinum.
2.1.2.3 Samples
2.1.2.3.1 Laboratory samples
Quartz glass samples for inspection shall not be contaminated on the surface and shall have a mass of not less than 10g. 2.1.2.3.2 Test samples
Proceed as in step 2.1.1.3.2.
2.1.2.4 Analysis steps
2.1.2.4.1 Test material
Weigh 3 portions of 0.1000g of the sample that has been dried at 105℃ for not less than 1h, accurate to 0.0001g, and place them in platinum. 2.1.2.4.2 Empty shot test
Except for not adding test material, the analysis steps, reagents and dosages are exactly the same as those for the determination, and the operation is carried out in parallel. 2.1.2.4.3 Determination of titanium dioxide
Moisten the sample in platinum with high-purity water, then add about 2 ml of sulfuric acid solution and 4 mL of hydrofluoric acid, evaporate at low temperature to 136°C on an electric furnace
GB/T 3284-93
Remove the remaining hydrofluoric acid, then raise the temperature again, and stop emitting white sulfur trioxide smoke after 10 minutes (do not evaporate too dry). After cooling slightly, transfer the test solution to a 300mL beaker, dilute to about 50mL with high-purity water, add 10.0mL 0.015mol./1.EDTA standard titration solution, heat for 40-50℃, add 1 drop of hemi-xylenol orange indicator, add ammonium hydroxide until the solution turns purple-red, and add a few drops of hydrochloric acid solution until the solution turns yellow. Heat and boil for 5min, cool, dilute to about 150mL with water, add 1g hexamethylenetetramine and 2-3 drops of hemi-xylenol orange indicator, add a few drops of hydrochloric acid solution until the solution turns yellow, and add zinc acetate solution until the solution changes from yellow to orange-red. 2.1.2.5 Expression of analytical results
The base content of titanium dioxide is expressed as its mass percentage, calculated according to formula (5): X = V/- (VV)alc × 79. 90
m × 1 000
Wherein: X-the percentage of titanium dioxide in the sample, %; V,-the volume of EDTA standard solution added, mL; V,~-the volume of zinc acetate solution consumed during titration, ml; -the volume of zinc acetate solution consumed when titrating the blank solution: X 100 ..
-Each liter of zinc acetate solution is equivalent to the volume of EDTA standard titration solution:-EDTA standard titration solution concentration.mol/I.;\Sample mass basis·",
79.90--Equivalent to the mass of titanium dioxide expressed in grams·g. The result should be expressed to two decimal places.
2.1.2.6 Allowable error
The allowable error of the analysis result is within 0.25%. 2.2 Emission spectrometry
2.2.1 The determined elements and the determination range are listed in Table 1. Table 1
Determined elements
2.2.2 Principle and method summary
2.2.2.1 Principle
Determination range
0. 03~3
0.003~0.3
C. 03 ~ 3
0. 003 0. 3
In the process of returning the excited state of the atom to the ground state, light of a specific wavelength is released. When the analysis conditions are fixed and the concentration of the element to be measured in the sample is relatively low, the intensity of the spectral line is proportional to the concentration of the element in the sample. 2.2.2.2 Summary of the method
GB/T 3284-93
Use hydrofluoric acid to decompose the sample, use the half-transfer method to transfer the sample solution to a pair of flat-head electrodes, evaporate and use the internal standard method, with palladium as the internal standard element. Use an AC arc to excite the sample. Determine using the spectroscopic analysis method. ·2.2.3 Reagents and materials
2.2.3.1 Hydrofluoric acid: high purity, 40% (V/V). 2.2.3.2 Hydrofluoric acid: 40% (V/V).
2. 2. 3. 3f Phosphate alcohol [CHOH(CHOH),CH,OH). 2.2.3.4 Glycol solution: Mannitol contains 5g/L. 2.2.3.5 Hydrochloric acid: high purity.
2.2.3.6 Nitric acid: high purity.
2.2.3.7 Internal standard solution:
2.2.3.7.1 Palladium internal standard concentrated solution: Palladium concentration is 1g/L. Weigh 0.1000g sponge palladium (spectral pure) to an accuracy of 0.0001g, place in a 150ml quartz glass beaker, add 2ml hydrochloric acid, 1ml nitric acid, dissolve under slight heat until the volume is close to 1. Add a few drops of water, then add about 1mL hydrochloric acid. Evaporate again until nearly dry. Add a small amount of water, and then add about 7ml hydrochloric acid. After the salts are dissolved, transfer to a 100ml volumetric flask and dilute to the scale with water. Sprinkle evenly. 2.2.3.7.2 Palladium internal standard dilute solution: Palladium concentration is 20mg/l. Take 2.0ml of palladium internal standard solution and place it in a 100ml volumetric flask, add 10ml hydrochloric acid and 0.1g potassium chloride (spectrally pure), dilute with water to the scale and shake.
2.2.3.7.3 Palladium internal standard dilution solution: Palladium concentration is 20mg/l. Take 5 ml of palladium internal standard concentrated solution and place it in a 250 ml volumetric flask. Add 24.5 ml of hydrochloric acid and 0.25 g of potassium chloride (spectrally pure). Dilute 1.25 g of bisphenol A with water to the mark. Shake well. 2.2.3.8 Mixed standard solution:
2.2.3.8.1 Lead standard solution: Concentration is 1 g/L. Weigh 250 g of aluminum powder (spectrally pure). Accurate to 0.0001, put it in a 150 ml beaker, add a little water and 25 ml of hydrochloric acid and dissolve it on an 80100 (electric furnace). After dissolution, cool it down and transfer it to a 250 ml volumetric flask. Dilute it with water to the mark. Shake well. 2. 2.3.8.2 Boron, magnesium, calcium, titanium, iron, cobalt, nickel mixed standard solution: boron concentration is 0.18/1. The concentrations of other elements are all 0.3g/L. Weigh 0.1129g of boric acid (spectrally pure), accurate to 0.0001g: 0.1244g of magnesium oxide (spectrally pure) burned to constant weight at 800 (accurate to 0.0001g: 0.1872g of calcium carbonate (spectrally pure) dried at 105-110 (dry for not less than 2h), accurate to 0.0001g; 0.1042g of potassium fluorotitanate (spectrally pure), accurate to 0.0001g: 0.1072g of calcium carbonate (spectrally pure) dried at 105-110 (dry for not less than 2h) h of ferric dioxide (spectrally pure), accurate to 0.(0001g: 0.0750g diamond sponge (spectrally pure), accurate to (.0001g: 0.0750g nickel sponge (spectrally pure), accurate to 00001; place in a 150ml quartz glass beaker. Add a small amount of water. Add 75ml of hydrochloric acid in several times, heat and dissolve in an electric furnace at 80~~90 (. After complete dissolution, cool and transfer to a 250mL volumetric flask and dilute with water to the scale, shake the hook. 2.2.3.8.3 Copper and manganese mixed standard solution: The concentration of copper and manganese is 0.03g/1 respectively. Weigh (.4164g silk 105~~110 (dry ← not less 2h of manganese tetraoxide (spectrally pure), accurate to 0.0001g: 0.3753g of copper oxide (spectrally pure) at 105-110 (dried for not less than 2h. Accurate to 0.0001%, placed in a 150ml quartz glass beaker, add a little water and 10ml. hydrochloric acid, dissolve with slight heat and cool. Transfer to a 100ml. volumetric bottle, dilute with water to the scale, shake 5.0ml of this solution. Add to 500)ml, put into a volumetric bottle, dilute to the scale with 10% hydrochloric acid. Shake well. 2.2.3.8.4 Mixed standard series solution:
a. First-level standard solution:
300 mg/1
Magnesium, calcium, iron, cobalt, nickel 30 mg/L each) Boron 10 mg/l.
Copper, manganese 3 mg/L each
Palladium 20 mg/l
GB/T 3284-93
Take 15.0mL aluminum standard solution (2.2.3.8.1) and 5.0mL two mixed standard solutions (2.2.3.8.2) and (2.2.3.8.3) in a 50mL volumetric flask, add 1mL palladium internal standard concentrated solution, 0.05g potassium chloride (spectrally pure) and 0.25g mannitol, dilute to the scale with palladium internal standard, and shake well.
b. Second level standard solution:
Aluminum 90 mg/1.
Magnesium, calcium, titanium, iron, cobalt, nickel 9 mg/L each Boron 3 mg/L
Copper, manganese 0.9 mg/L each
Palladium 20 mg/1.
Take 15.0mL of the first level standard solution (item a in 2.2.3.8.4), place it in a 50mL volumetric flask, and dilute it to the mark with palladium diluent. c.
The third level standard solution is diluted 10 times with palladium diluent from the first level standard solution. The fourth level standard solution is diluted 100 times with palladium diluent from the first level standard solution. The fifth and sixth level standard solutions are diluted 10 times with palladium internal standard diluent from the third and fourth level standard solutions, respectively. Note: (i) The above standard solutions and mixed standard series solutions are stored in polyethylene plastic bottles. (② The standard series differential concentration and the amount of internal standard elements added can be appropriately changed according to different instruments. 2.2.3.9 Sealing agent: polystyrene, concentration is 10g/L. Weigh about 1g of polystyrene (analytical grade) and place it in a glass bottle, add 100mL of ethyl acetate (analytical grade) to dissolve. 2.2.3.10 Developer
Solution A: 2g/L of p-methylaminophenol sulfate (Metol), 52g/L of anhydrous sodium sulfite, 10g/L of hydroquinone; Solution B: 44g/L of anhydrous sodium carbonate, 2g/L of potassium bromide; when using, mix A and B solutions in a 1+1 ratio.
2.2.3.11 Stop solution: 3%~~6% glacial acetic acid solution; 2.2.3.12
Fixing solution: sodium thiosulfate 400g/L, anhydrous sodium sulfite 25g/L, glacial acetic acid 8×103% (V/V); high-purity water: secondary exchange water;
1 Graphite electrode: spectrally pure, diameter 6mm; 2.2.3.14
Photosensitive plate: UV type I;
Platinum crucible:
Organic glass operating box (with infrared lamp); 2.2.3.18
3 Stone decomposition box: high-purity graphite.
2.2.4 Instruments and equipment
2.2.4.1 Emission spectrograph: three-lens illumination system prism or grating spectrograph; 2.2.4.2 AC arc generator: 380V, 8A; 2.2.4.3 Microphotometer: sensitivity 2.5×10-3A/mm/m, vibration period approximately equal to 1s: 2.2.5 Samples
2.2.5.1 Laboratory samples
Quartz glass and high-purity quartz glass samples for inspection must keep the surface clean, without graffiti and dirt scratches, and the crystal raw materials and silica samples must be uniform. The sample mass is not less than 50g. 2.2.5.2 Samples
Proceed according to the steps in 2.1.1.3.2.
2.2.6 Analysis steps
2.2.6.1 Test material
Weigh about 0.2g of the sample, accurate to 0.0001g, and place it in a platinum crucible, and perform three parallel operations. 2.2.6.2 Blank test
GB/T 3284--93
Except that no test material is added, the analysis steps, reagents and dosages are exactly the same as those for the determination. Perform parallel operations. 2.2.6.3 Determination
2.2.6.3.1 Add 0.1ml of mannitol solution and a little basic water to the crucible containing the test material to moisten it. Place the crucible on the grid plate of the graphite box [150mL of hydrofluoric acid (2.2.3.2) and 1g of mannitol are added to the bottom of the box in advance] and cover the box lid. Heat the upper and lower parts of the box with an electric furnace, and keep the temperature in the box at 105-110°C (2.5-3h). If high-purity hydrofluoric acid is used to directly decompose the sample, add 3-4mL of hydrofluoric acid (2.2.3.1) to the crucible, cover the crucible, and heat it with an electric furnace for about 1.5h). After the sample is completely decomposed, take out the crucible and evaporate it to dryness on an 80-100°C electric furnace, and cool it.
2.2.6.3.2 Add 0.2mL of dilute palladium internal standard solution to the crucible and diffuse the residue. Pipette 0.1mL of this solution and transfer it to the top of a pair of flat-head electrodes coated with 1 drop of sealing agent, evaporate it to dryness under an infrared lamp, and wait for spectrum photography. 2.2.6.3.3 Take 0.1mL of the mixed standard series solution and transfer it to the top of a pair of flat-head electrodes coated with 1 drop of sealing agent, evaporate it to dryness under an infrared lamp, and wait for spectrum photography.
2.2.6.3.4 Take the standard series solution, sample and blank on the same spectrum plate under the same spectrum conditions as below. 2.2.6.3.5 Spectral conditions: Use emission spectrometer to take the spectrum, and its slit and intermediate grating are customized according to the instrument model. AC arc 8A, exposure 30s (no pre-burning).
2.2.6.3.6 Develop the spectrum plate at 20±1C for 4min, stop for 15~20s, fix for 10~20min, wash with water for about 20min and dry.
2.2.6.3.7 Use microphotometer to measure the blackness of the analytical line pair. 2.2.6.3.8 Analytical line and internal standard line
2.2.6.3.8.1 Analytical line (nm)
B 1249. 77; Mg 1277. 98; A1 1266. 03; Ca 11317. 93; Ti I1308.80; Mn 1279.82; Fe I1259. 95; Co1304.40;Ni 1305.08;Cu 1327.39.2.2.6.3.8.2 Internal standard line (nm)
Pd 1 302. 79
2.2.6.4 Drawing of working curve
Use the blackness value of the analytical line pair of the standard series measured in 2.2.6.3.7 and the concentration value of the standard solution to draw the AW-1gC working curve. 2.2.7 Expression of analysis results
2.2.7.1 The analysis results are expressed in percentage (%). 2.2.7.2 The analysis results are calculated according to formula (6): m×10%×100
-the percentage content of the element to be measured in the sample, %; where: X,-
-the actual content of the element to be measured in the sample and the sum of the blank value, g: blank value, ug;
the mass of the sample·g.
The result should be expressed to two decimal places.
2.2.8 Precision
The relative standard deviations of different base content ranges are listed in Table 2.140
Content range
10～300
The relative standard deviation of Table 2 is calculated according to formula (7): Where: r-—→relative standard deviation, %; c-—average concentration, mg/L;
d——difference between measured value and average value, mg/L; number of measurements.
The results should be expressed to two decimal places.
2.3 Graphite furnace atomic absorption spectrometry
GB/T 3284—93
2.3.1 The elements to be measured and the range of measurement are listed in Table 3. In case of dispute, this method shall prevail. Table 3
Determination elements
2.3.2 Principle
Determination range
5～100
5～100
Determination elements
Relative standard deviation
25(B≤15)
Determination range
5～100
Gaseous atoms can selectively absorb light of a specific wavelength, and the degree of absorption is linearly related to the concentration of the element to be measured in the solution. 2.3.3 Reagents and materials
2.3.3.1 Hydrofluoric acid: high purity,
Hydrochloric acid: high purity.
2.3.3.3 Nitric acid: high purity.
Nitric acid solution: 1% (V/V), prepared with nitric acid (high purity) when used. 2.3.3.5 Mixed standard solution.
Aluminum standard solution: aluminum concentration is 1mg/mL. (7)
Weigh 1.0000g of aluminum chips (99.999%), accurate to 0.0001g, place in a 200mL quartz glass beaker, add 20ml of hydrochloric acid 141
GB/T3284—93
, 5ml of nitric acid, heat to dissolve, cool and transfer to a 1000mL volumetric flask, add 80ml of hydrochloric acid, dilute to the mark with high-purity water, and shake well. Transfer the solution to a polyethylene plastic bottle for storage. b. Iron standard solution: iron concentration is 1mg/mL. Weigh 1.0000g of iron wire (spectrally pure) to the nearest 0.0001g and place it in a 200ml quartz glass beaker. Add 30ml of nitric acid (1+1. high purity) and heat to dissolve. Heat until almost dry to drive out all nitrogen dioxide. Add 20mL of hydrochloric acid. After cooling, transfer to a 1000ml volumetric flask, dilute to scale with high-purity water, and shake well. Transfer the solution to a polyethylene plastic bottle for storage. c. Magnesium standard solution: magnesium concentration is 1mg/mL. Weigh 1.6580g of magnesium oxide (spectrally pure) burned to constant weight at 800C to the nearest 0.0001g and place it in a 200ml quartz glass beaker. Add 20mlL of high-purity water and then slowly add 20mL of hydrochloric acid. After it is completely dissolved, heat and boil to drive out all carbon dioxide. After cooling, transfer to a 1000ml volumetric flask, dilute to scale with high-purity water, and shake well. Transfer the solution to a polyethylene plastic bottle for storage. d. Calcium standard solution: Calcium concentration is 1mg/mL. Weigh 2.4972g of calcium carbonate dried at 105-110C for not less than 2h, accurately to 0.0001g, cover in a 200ml quartz glass beaker. Add 20ml of high-purity water and drop hydrochloric acid (1+1, high-purity) until completely dissolved, then pass through 10ml of hydrochloric acid, boil to remove carbon dioxide, cool and transfer to a 1000ml volumetric flask. Dilute to scale with high-purity water and shake well. Transfer the solution to a polyethylene plastic bottle for storage. e. Titanium standard solution: Titanium concentration is 1mg/ml. Weigh 1.0000g of titanium powder (spectrally pure), accurately to 0.0001g, cover in a 200ml quartz glass beaker, add 100mL of hydrochloric acid and heat until completely dissolved, then cool. Transfer to a 1000mL volumetric flask, dilute to scale with 10% hydrochloric acid and shake well. Transfer the solution to a polyethylene plastic bottle for storage. e. Titanium standard solution: Titanium concentration is 1mg/ml. Weigh 1.0000g of titanium powder (spectrally pure), accurately to 0.0001g, cover in a 200ml quartz glass beaker, add 100mL of hydrochloric acid and heat until completely dissolved, then cool. Transfer to a 1000mL volumetric flask, dilute to scale with 10% hydrochloric acid and shake well. Transfer the solution to a polyethylene plastic bottle for storage.
f. Nickel standard solution: Nickel concentration is 1mg/mL. Weigh 1.2726g of nickel oxide (spectrally pure) that has been dried at 110°C for not less than 2h, accurate to 0.0001g, place in a 200mL quartz glass beaker, add 15ml hydrochloric acid and 5ml nitric acid, heat to dissolve, and heat to drive out nitrogen dioxide.After cooling, transfer to a 1000mL volumetric flask, dilute to the mark with high-purity water, and shake well. Transfer the solution to a polyethylene plastic bottle for storage. g. Manganese standard solution: manganese concentration is 1mg/mL. Weigh 1.3884g of manganese tetraoxide (spectrally pure) dried at 110C, accurately to 0.0001g, place in a 200mL quartz glass beaker, add a small amount of high-purity water and 30mL hydrochloric acid, dissolve with slight heat, cool and transfer to a 1000mL volumetric flask, dilute to the mark with high-purity water, and shake well. Transfer the solution to a polyethylene plastic bottle for storage. h. Cobalt standard solution: cobalt concentration is 1 mg/mL. Weigh 1.3620g of cobalt tetraoxide (spectrally pure) dried at 110C, accurately to 0.0001g, place in a 200ml quartz glass beaker, add 20ml high-purity water and 25mL hydrochloric acid, and heat to dissolve. If the solution dissolves slowly and evaporates to near dryness, add an appropriate amount of hydrochloric acid. After complete dissolution, cool it, transfer it to a 1000mL volumetric flask, dilute it to the mark with high-purity water, and shake it well. Transfer the solution to a polyethylene plastic bottle for storage. i. Copper standard solution: The copper concentration is 1mg/mL. Weigh 1.2518g of copper oxide (high purity) that has been dried at 110C for not less than 2h, accurate to 0.0001g, place it in a 200mL quartz glass beaker, add low-base high-purity water and then 30mL of hydrochloric acid, dissolve it with slight heat, cool it, transfer it to a 1000ml volumetric flask, dilute it to the mark with high-purity water, and shake it. Transfer the solution to a polyethylene plastic bottle for storage. j. Lithium standard solution: The lithium concentration is 1mg/mL. Weigh 5.3252g of lithium carbonate (high purity) dried at 110°C for not less than 2h, accurate to 0.0001g, and place in a 200mL quartz glass beaker. Add 50mL high-purity water and 20mL nitric acid (1+1, high purity), heat and boil to remove carbon dioxide after dissolving, cool and transfer to a 1000ml container, dilute to scale with high-purity water, and shake well. Transfer the solution to a polyethylene plastic bottle for storage. k. Sodium standard solution: Sodium concentration is 1mg/mL. Weigh 2.4520g of sodium chloride (spectrally pure) that has been burned for not less than 1h at 600°C, accurate to 0.0001g, and place it in a 200ml quartz glass beaker. Add 50ml of high-purity water and 20mL of nitric acid (1+1, high-purity), dissolve it and transfer it to a 1000mL volumetric flask, dilute it to the mark with high-purity water, and shake it well. Transfer the solution to a polyethylene plastic bottle for storage. 1. Potassium standard solution: The potassium concentration is 1mg/mL. 142
GB/T 3284—93
Weigh 1.9072g of potassium chloride (spectrally pure) that has been burned at 600C for not less than 1h, accurate to 0.0001g, place in a 200mL quartz glass beaker, add 50mL high-purity water and 20mL nitric acid (1+1. high-purity), transfer to a 1000mL volumetric flask after dissolving, dilute to the mark with high-purity water, and shake. Transfer the solution to a polyethylene plastic bottle for storage. Mixed standard solution:
Iron, magnesium, calcium, titanium, lithium, sodium, potassium
Nickel, manganese, copper, cobalt
20μg/mL
10 μg/mL
5μg/mL
Pipette 400mL of aluminum standard solution obtained in item a; 2.00mL of iron, magnesium, calcium, titanium standard solutions obtained in items b to e and 2.00mL of lithium, sodium, potassium standard solutions obtained in items i to 1; 1.00mL of nickel, manganese, cobalt, and copper standard solutions obtained in items f to i into a 200mL container, add 4mL of nitric acid, cool, dilute to scale with high-purity water, and shake well. Transfer the solution into a polyethylene plastic bottle. Store in a material bottle for future use. n. Standard series solution
Take 0.100.20, 0.40, 0.60, 1.00, 1.40.1.80, 2.00.4.00.6.00ml of the mixed standard solution obtained in item m respectively in a 200mL container, add 2ml of nitric acid, dilute to the scale with high-purity water and shake well. The concentrations of this solution are: 5, 10, 20.30, 50.70, 90.70, 10 ... 0, 100ug/L; nickel, manganese, copper, cobalt are 2.5, 5.10, 15, 25.35, 45.50g/L respectively; aluminum are 10, 20.40, 60, 100.140, 180, 200, 400, 600μg/L respectively. 2.3.3.6 High-purity water: secondary exchange water.
2.3.3.7 Platinum.
2.3.3.8 Graphite decomposition box: high-purity graphite. 2.3.4 Instruments and equipment||t t||2.3.4.1 Stone furnace atomic absorption spectrometer. 2.3.4.2 Iron, magnesium, calcium, aluminum, titanium, nickel, manganese, copper, cobalt, lithium, sodium, potassium hollow cathode lamp. 2.3.4.3 Electric furnace 2000W.
2.3.5 Samples
2.3.5.1 Laboratory samples
Proceed according to the steps of 2.2.5.1.
2.3.5.2 Samples
Proceed according to the steps of 2.1.1.3.2.
2.3.6 Analysis steps
2.3.6.1 Samples
Weigh 0.05~0.1g of sample (depending on the impurity content) dried at 105~110℃ for not less than 2h, accurate to 0.0001g, and place in a platinum crucible, in triplicate.
2.3.6.2 Blank test
Except that no sample is added, the same analytical steps, reagents and dosages as those for the determination are used for parallel operation. 2.3.6.3 Determination
2.3.6.3.1 Sample solution
Add a small amount of high-purity water to the platinum crucible containing the sample to wet the sample, then add 2~3mL of hydrofluoric acid, place the platinum crucible on the grid plate in the graphite decomposition box, cover the crucible cover and the graphite decomposition box cover, place the graphite decomposition box on an electric furnace for heating, and adjust the furnace voltage to 100~130V (depending on the ambient temperature). After 1.5h, take out the crucible, place it on an opaque quartz plate (or asbestos mesh), and slowly heat and evaporate it to dryness to drive out all the hydrofluoric acid. After the crucible is removed and cooled, add 10mL of nitric acid solution, shake it evenly after it is completely dissolved, and then test it. 2.3.6.3.2 Working curve method
Instrument parameters
GB/T 3284—93
Lamp current
Instrument working conditions)
Drying temperature
Note: 1) The parameters in the table are only applicable to this instrument, and other instruments should be determined separately. Ashing temperature
Atomic flower
Treatment temperature
Set the working conditions of the stone furnace atomic absorption spectrometer according to the parameters shown in Table 4, select three mixed standard solutions (2.3.3.5) according to the element concentration range determined by the sample solution, and automatically calibrate the instrument. Program the blank solution and the sample solution, and determine the concentration values of iron, magnesium, calcium, aluminum, titanium, nickel, manganese, copper, cobalt, lithium, sodium, and potassium in the blank solution and the sample solution in turn. When the spectrometer cannot be automatically calibrated, the absorbance of each element in the blank solution and the sample solution can be determined. Then, the concentration values of each element in the blank solution and the sample solution are found from the concentration-absorbance (CA) working curve obtained in 2.3.6.4. 2.3.6.3.3 Tight interpolation method
Set the working conditions of the atomic absorption spectrometer according to the parameters shown in Table 4, program the test solution, blank solution and standard solution, and use the tight interpolation method to determine the absorbance of iron, magnesium, calcium, aluminum, titanium, nickel, manganese, copper, cobalt, lithium, sodium and potassium. 2.3.6.4 Drawing of working curve
Determine the absorbance of each element of iron, magnesium, calcium, aluminum, titanium, nickel, manganese, copper, cobalt, lithium, sodium and potassium in the standard series solution according to the steps in 2.3.6.3.2. Then draw the concentration-absorbance (CA) working curve using the concentration of the standard solution and its measured absorbance. 2.3.7 Expression of analysis results
2.3.7.1 The analysis results are expressed in percentage (%). 2.3.7.2 Working curve method: When the working curve method is used for determination, the content of the measured element in the sample is calculated according to formula (8): X = X-
% of the measured element, %; (Cx-c,)Vm × 10°
Concentration of the measured element in the sample solution, g/I.; × 100
(8) GB/T 3284-93 (--Concentration of the measured element in the blank solution, μg/L; ---Volume of the sample solution, mL; m -mass of the sample·g. 2.3.7.3 Close interpolation method: When the close interpolation method is used for determination, the content of the measured element in the sample is calculated according to formula (9): X = [C, +BD
Cz Ci
m×10° × 100
×(Dx D,)|×
Wherein: X. Percentage of the element being measured, %; C1, C2—concentrations of two standard solutions·μg/L, I),、D2—absorbance of one or two standard solutions; Dx—absorbance of the sample solution;
V—volume of the sample solution, mL;bZxz.net
—mass of the sample, g.
2.3.7.4 The results obtained by the working curve method and the close interpolation method should be expressed to two decimal places. 2.3.8 Precision
The relative standard deviations of the measurements in different content ranges are listed in Table 5. Table 5
Content range
10～100
1～10
0. 01～0. 1
2.4 Flame atomic absorption spectrometry
2.4.1 Determination of elements
Sodium, potassium, lithium.
2.4.2 Principle
See 2.3.2.
2.4.3 Reagents and Materials
2.4.3.1 Chloride: spectrally pure.
Hydrofluoric acid: high purity, 40% (V/V).
2.4.3.3 Hydrofluoric acid: 40% (V/V).
Nitric acid solution: 1% (V/V), prepared with nitric acid (high purity) when used. 2.4.3.5 Lithium, sodium, potassium mixed standard solution: lithium, sodium, potassium concentrations are all 1g/L. Mixed concentrated standard solution: lithium, sodium, potassium concentrations are all 1g/L. a.
Relative standard deviation
.....(9)
Weigh 1.3308g of lithium carbonate (spectrally pure) dried at 110°C for not less than 2h, accurate to 0.0001g; 0.6355g of sodium pyrochlore (spectrally pure) calcined at 600°C for not less than 1h, accurate to 0.0001g; 0.4768g of potassium chloride (spectrally pure) calcined at 600°C for not less than 1h, accurate to 0.0001g, put them in the same 150mL quartz glass beaker, add about 50mL of water and 5mL of nitric acid, dissolve, heat to boil to remove carbon dioxide, cool, transfer to a 250mL volumetric flask, dilute to scale with water, and shake well. Transfer the solution to a polyethylene plastic bottle for storage.
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