Some standard content:
Electronic Industry Standard of the People's Republic of China
SJ/T10461-93
Strontium Carbonate for Use in Electronic Glass
Strontium Carbonate for USC in Electronic Glass1993-12-17Published
1994-06-01Implementation
Published by the Ministry of Electronics Industry of the People's Republic of China
Strontium Carbonate for Use in Electronic Glass
Strontium Carhonate for Use in Eleetrunie GlassSubject Content and Scope of Application1.1 Subject ContentSJ/T 10461-93
This standard specifies the technical requirements, inspection methods, marking, packaging, transportation and storage of strontium carbonate for use in electronic glass. 1.2 Scope of ApplicationThis standard is applicable to strontium carbonate for use in electronic glass (hereinafter referred to as carbonate mixture). 2 Reference standards
GB9000.1 General principles for chemical analysis of electronic glass 3 Technical requirements
3.1 Appearance
Strontium carbonate is white or slightly yellowish fine particles, and should be free of mechanical inclusions. 3.2 Particle size
The particle size distribution of strontium carbonate is shown in Table 1
Particle size (mm)
Note: If there are special requirements for particle size, it shall be agreed upon by the supplier and the buyer. 3.3 Chemical composition
The chemical composition of strontium carbonate is shown in Table 2.
Approved by the Ministry of Electronics Industry of the Republic of China on December 17, 1993 Ratio (%)
Implemented on June 1, 1994
Strontium phosphate (SRCx))
Barium carbonate (RaCO)
Calcium carbon (CaC)
Total iron (in Fe0,)
Total road (in Cr2,)
Total phosphorus (in P,;
Total chlorine (in L)
Total (CO)
Total plating (in O)
Total Mn (in Mn)
3.4 Submersible
The water content of carbonate saws should be less than 0.3%
4 Inspection method
4.1 Appearance: daylight method.
4.2 Determination of particle size distribution
4.2.1 Instrument and sample
a. Vibrating screen (excavator);
SJ/T 10461 -- 93
Standard sieves 1.46, 0.840, 0.210, 0.105mmb.
Sieve base, cover and hairline;
d. Test selection and verification at 100t Bake for 1 hour, take 100g for testing. 4.2.2 Determination method
Content range (%)
(1) Test the standard sieve, which should be free of any holes and fit tightly. Use wool to carefully clean the sieve before testing to remove any sticky residue.
(2) Place the standard sieves in the order of 1.410, 0.B40, 0.210, 0.105mm, and the sieve seat from top to bottom, place 100g of the sample in the 1.410mm sieve, cover the sieve cover, and then place the standard sieve on the vibrator, tighten it. Clamp. (3) Set the timer to 15 minutes and start the vibrator until the vibration stops. (4) Use a brush to gently move each sieved material onto white paper. Do not let it fall. 4.2.3 Calculation of results
Calculate the percentage of each sieve based on the weighing result and the total weight. The weighing of the entire analysis process should be accurate to 0.1ge. Note: ① Each sieve should be effectively leveled during sieving. The sieve is dried in a 10-degree oven. 4.3 Determination of the chemical composition of strontium carbonate
The relevant regulations for the determination of the chemical composition of strontium carbonate shall comply with the requirements of GB 9000.1. 4.3.1 Determination of strontium carbonate
4.3.1.1 Key points of the method:
SJ/T 10461-93
The sample is decomposed with hydrochloric acid to remove all carbon dioxide and then eluted with EDTA at a pH of 10. Titrate the contents of strontium, barium and calcium, deduct the barium and calcium measured by atomic absorption spectrometry, and the remainder is the content of strontium carbonate. 4.3.1.2 Reagents and solutions
a. Hydrochloric acid;
b. Hydrochloric acid: (2+1);
c. Ammonia water;
buffered solution (PHα10)
Weigh 70g of ammonium chloride and dissolve it in appropriate amount of water, add 570ml of ammonia water, and dilute to 1000ml with water; e. Methyl benzyl alcohol (MTB) ,0.1%：f. Black T,1%
Dissolve 10g of Chrome Black T in 75ml of triethanolamine and 25ml of ethanol, and store in a brown bottle: g Zinc standard solution, C(ZaCl,)=0.05mol/L Weigh 1.6343g of pure zinc (99.99% or more), add about 50ml of water, 10ml of hydrochloric acid (2+1), 10 drops of water, heat to dissolve, boil slightly for a while to drive out the bromine water, cool and transfer to a 500ml volumetric flask, dilute to scale; h. EDTA standard solution, C(EDTA) =0.05mol/L Weigh 18.7g of disodium ethylenediaminetetraacetate and dissolve in an appropriate amount of water, adjust the pH to 5 with 10% sodium hydroxide solution, dilute to 1000ml with water, shake and set aside.
【Calibration】Accurately pipette 25ml of zinc standard solution into a 300ml conical flask, add 70ml of water. Use 20% sodium hydroxide solution to neutralize the room pH to 6~7. Add 10ml of buffer solution, use chrome black T as an indicator, and titrate with EDTA standard solution until the solution changes from wine red to pure blue, and calculate the concentration of EDTA standard solution. 4.3.1.3 Analysis steps
Weigh 2.00g of the sample into a 200ml beaker, add 50ml of water and 5ml of hydrochloric acid, cover, heat to dissolve, and drive out carbon dioxide. After cooling, add about 100ml of water (leave overnight), filter with slow filter paper, fully wash the insoluble matter and filter paper, collect the filtrate and wash in a 250ml volumetric flask, and dilute to the scale. Shake well. Pipette 25 ml of the test solution into a 300 ml blue flask, add 20 ml of nitrogen water, 10 ml of buffer solution, a little methyl muscovado blue indicator, add water to 100 ml and titrate with EDTA standard solution until the solution turns gray. 4.3.1.4 Calculation of results
The content of strontium carbonate in the sample is calculated according to the following formula: StC0 = M ×yXV476x 100 ×10 - 0.748 × 3acCO,% -1.475 x Cac0, % 10
Wherein: M——concentration of EDTA standard solution, MOL/LV——volume of EDTA standard solution consumed during titration, mlW sample weight;
BaCO,%——content of sodium carbonate;
Ca,%——content of calcium carbonate;
SJ/T10461-93
0.748——conversion coefficient of carbonic acid to sodium carbonate; 1.475——conversion coefficient of calcium carbonate to strontium carbonate; 147.6~the mass of strontium carbonate.
4.3.2 Determination of calcium carbonate and barium carbonate (AAS method) 4.3.2.1 Key points of the method
The sample is dissolved in hydrochloric acid medium, carbon dioxide is driven out, and the atomic absorbance of calcium barium is determined by atomic absorption spectrometry according to the analytical conditions.
4.3.2.2 Reagents and solutions
a. Hydrochloric acid;
h Hydrochloric acid, (1+1);
c. Standard solution of calcium carbonate (equivalent to 1.2 mg/ml of calcium carbonate) Accurately weigh 2.22 g of anhydrous calcium oxide (standard), dissolve it in water, transfer it into a 500 ml volumetric bottle, dilute to the scale (equivalent to 4 mg/ml of CeCOg), and dilute the solution 20 times as a standard solution of calcium carbonate. "Calibration 1 Take 20ml of chlorinated solution (equivalent to containing 4mg/ml of CaCO) and put it in a 300ml diagonal bottle. Use 20% sodium hydroxide solution to adjust the H value to 10. Use calcium reagent (NN) to indicate the end point. Titrate with 0.05M EDTA standard solution until the solution changes from red to pure, and calculate the concentration of calcium carbonate standard solution. d. Carbon barium standard solution [equivalent to containing 2mg/ml of barium carbonate] Take 2.11g of chlorinated sodium carbonate over 105C dry coal and dissolve it in water. Add 1ml of blue acid (1!1), transfer it to a 1000ml volumetric flask and dilute to the scale. (The accurate concentration can be calibrated by barium sulfate weight method): e: Potassium oxide solution (containing potassium (K-) 4mg/ml) Weigh 7.6g of potassium chloride and dissolve it in 1000ml of water. 4.3.2.3 Analysis steps
a.Take 5 100ml volumetric flasks and prepare the standard series solution according to the requirements of Table 3. Table 3 Standard series solution
Sample sample volume\Addition amount (ml)
Calcium carbonate standard solution addition amount (ml)
Calcium carbonate standard solution addition amount (zml)
Potassium chloride solution addition amount [ml]
Note: 1) The preparation of the sample solution shall refer to 4.3.1.3 of this standard. 10
b. According to the test conditions listed in Table 4, measure the atomic absorption intensity of calcium and sodium in the standard series solution. Table 4 Conditions for determination of calcium and steel by AAS method
Leveling line
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Length (ert)
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Flame type
Air-acetylene
Nitrogen oxide-acetylene
Gas flow rate (1./min)
Combustion-aiding gas
Combustible gas
Based on the measured atomic absorbances of calcium and barium carbonate in the standard series of solutions 1 to 5, the contents of calcium carbonate and barium carbonate in the strontium sulfonate sample are calculated by the standard addition method according to the requirements of Section 4.3.2.4. 4.3.2.4 Calculation of results
SJ/I 1046193
4.3.2.4.1 Calculate the atomic absorbance of the standard series solutions No. 1 to 5, plot the relationship between the calcium and barium contents and their atomic absorbance, and use the extrapolation method to draw a graph to calculate the content of calcium carbonate and barium carbonate in 10 ml of the sample solution (mg). 4.3.2.4.2 The content of calcium carbonate (or carbon dioxide) in the sample is calculated according to the following formula: mx25
CacOg(or BaCOs)=
W×1000
Wherein: m—the amount of calcium carbonate (or barium carbonate) in the test solution, mg; W—the sample weight, g.
4.3.3 Determination of Sulfur
4.3.3.1 Key points of the method
The sample is dissolved in a mixed flux of sodium carbonate and potassium nitrate, leached in water, so that sulfur remains in the solution in the form of sulfate, and then precipitated with barium chloride solution and quantified by weight method. 4.3.3.2 Reagents and solutions
Anhydrous sodium carbonate;
Nitric acid;
Sodium carbonate solution 0.2%;
Hydrochloric acid, (1+1):
Barium chloride solution, 10%;
Methyl red solution, 0.1% ethanol solution.
4.3.3.3 Analysis steps
Accurately weigh 1.Dg of the sample in a platinum dish, add 4g of anhydrous sodium carbonate and 0.1g of potassium nitrate, and mix well. Add 1.0g of anhydrous sodium carbonate to cover it, heat and melt until clear, continue for 5 minutes, cool and add 40ml of water, dissolve the gold in a water bath, filter with slow filter paper, wash several times with 0.2% sodium carbonate solution. Wash with warm water 3-4 times, collect the filtrate and washing liquid in a 300ml beaker, add 2 drops of methyl line indicator. Cover with a watch glass, carefully add hydrochloric acid (111) to neutralize, then add 5tnl in excess, boil to drive out carbon dichloride. Move it to a water bath. Add 10ml of 10% barium chloride solution dropwise under vigorous stirring, keep warm for 1h, and place it warm for 4-6h or overnight.
Filter with slow fixed base filter paper, wash with warm water until there is no nitrogen ion, place the precipitate and filter paper together in a constant weight increase, dry, ash, and then keep it at B00C for 30min, cool in a desiccator, and weigh to constant weight. 4.3.3.4 Calculation
The sulfur content in the sample (in terms of $) shall be calculated according to the following formula: mx.0.343x100
W ×1000
W—weight of sulfuric acid precipitate (difference between two weighings), mg 0.343—conversion coefficient of sulfuric acid to sulfur trioxide: W—sample weight, g:
4.3.4 Determination of iron
...+..(3)
4.3.4.1 Key points of the method
SJ/T10461-93
Dissolve the sample in acid and reduce the iron with hydroxylamine hydrochloride in a weakly acidic medium. Use o-phenanthroline to react with divalent iron to form a red complex for spectrophotometric analysis.
4.3.4.2 Reagents and solutions
Hydrochloric acid, (I+1)bzxZ.net
Ammonia water, (I+1);
Alcoholic acid solution, 10%:
d. Hydroxylamine hydrochloride solution, 10%,
O-phenanthroline solution. 0.1%:
"P-nitrophenol (PNP) solution, 0.2%:
g. Standard solution of iron oxide, containing 0.03mu/ml of ferric oxide. Weigh 0.3000g of ferric oxide, such as 10ml of hydrochloric acid (1-1), heat to dissolve, and then dilute to 500ml, dilute 20 times when used (containing 0.03mg/ml of ferric oxide). 4.3.4.3 Analysis Steps
Weigh 10g of the sample into a 200ml beaker, add 50ml of water and 25ml of hydrochloric acid (1+1), heat to dissolve, and leave for several hours a.
or overnight.
Filter through filter paper, wash with hot water 3~4 times, collect the filtrate and washings in a 250ml volumetric flask, dilute to scale, b. Pipette 25ml of the above solution into a 100ml volumetric flask, add 5ml of tartaric acid solution, 2 drops of PNP indicator, adjust the pH value with ammonia water [1+1) until the solution turns yellow. Then adjust to colorless with hydrochloric acid (1+1), 2 drops in excess. Add water to about 80ml, add 2ml of hydroxylamine hydrochloride and 10ml of o-phenanthrin solution, shake well and dilute to scale, leave for 30min and measure the absorbance. c. Accurately pipette 0, 1, 2, 34, 5 ml of the standard solution of iron oxide into 100 ml volumetric flasks respectively, dilute to 25 ml with water, and prepare the standard solution series according to Section 4.3.4.3h. d. Measure the absorbance at 51 nm wavelength of the spectrophotometer with the sample blank as the control. 4.3, 4.4 Result calculation
4.3.4.4.1 Draw the standard working curve based on the measured absorbance of the standard series solution, and find out the content of ferric oxide in the test solution from the standard working curve according to the absorbance of the sample solution. 4.3.4.4.2 The content of ferric oxide in the test solution is calculated as follows: m×10
Fe2O, % =
W×1000
Wm-the amount of ferric oxide in the sample solution, g; Wm-the amount of sample, g
4.3.5 Determination of chromium
4.3.5.1 Method requirements
+* (4)
After the sample is melted, separate the insoluble sulfate in sulfuric acid medium, decompose the chromium with potassium permanganate to make all the chromium in a hexavalent state, use carbazine to form a colored complex with hexavalent chromium, and quantify it by spectrophotometry. 4.3.5.2 Reagents and solutions
a. Hydrochloric acid (1+1);
b. Sulfuric acid (1+1);
c. Potassium permanganate solution, 0.5%;
d. Urea solution, 20%;
Sodium sulfite solution, 10%;
[Sodium nitrite solution, 10%;
g: Ferric sulfate solution (containing iron [mg/ml) SJ/T 10461-93
Weigh 0.864 ml of ammonium ferric sulfate, add 50 ml of water, 5 ml of sulfuric acid (1+1), dissolve and transfer into a 100 ml volumetric flask, dilute to 1 h, diphenylcarbazine (C3I14N.0), 0.2% ethanol solution, place in a brown bottle, store at the spectrum: i. Chromium oxide standard stock solution (containing chromium trioxide 100ug/ml) Weigh 0.1936g of potassium dichromate (standard) in a beaker, add water to dissolve, transfer to a 1000ml volumetric flask, dilute to scale;
j. Chromium oxide standard solution (containing chromium trichloride 2.5μg/ml) Pipette 25ml of chromium oxide stock solution in a 1000ml volumetric flask, dilute to scale with water. 4.3.5.3 Analysis steps
a: Accurately weigh 1~2g of the sample in a 300ml beaker, add 60ml of water, add 20ml of hydrochloric acid (1+1), heat to dissolve 1), and boil to drive out all carbon monoxide. Add 0.5ml of sodium sulfite solution, boil slightly for a while, add 10ml of sulfuric acid (1+1) dropwise while stirring constantly, and keep it on a water bath for 30min. Remove and cool, filter with slow filter paper, wash the sulfuric acid melt (1+9) 2~-3 times, wash with water several times, remove the precipitate, and collect the filtrate and washing liquid in a 300ml flask. Note: 1) If the solution is not completely clear, filter with medium-speed shaking paper, wash with 1+99) hydrochloric acid 2~3 times, dry the filter paper and the residue, incinerate, and melt with 2g of anhydrous sodium ferric sulfate and 1.1g of potassium nitrate. After the melt is dissolved with hydrochloric acid (1+1), add it to the filtrate and perform the following operation. b: Heat the melt on a sand bath to evaporate until white sulfuric acid smoke is generated and lasts for about 3min, cool to room temperature, and add about 70ml of water.2 drops of p-nitrophenol indicator, adjust to yellow with ammonia water, then adjust to colorless with sulfuric acid (1+1), and add 3ml excess, add 4ml of ammonium ferric sulfate solution, heat on an electric stove until slightly boiling, add potassium permanganate solution until purple (about 2ml), boil, make the melt volume about 60ml, cool, add 10ml of 20% urea solution, shake well. Add sodium nitrite solution until the purple color of potassium permanganate just disappears, stir vigorously to remove all bubbles, transfer to a 100ml volumetric flask after cooling, add 2ml of diphenylcarbazide solution, use a spoon, dilute to the scale, and measure the absorbance of the standard series solution at the wavelength of 540nm on a spectrophotometer for 5min. At the same time, do a blank test for the sample.
C. Standard working curve
Pipette 0, 2...5 ml of chromium oxide standard solution into 200 ml beakers respectively, add water to 70 ml, add 2 drops of phenol indicator, and perform the following operations according to 4.3.5.36 of this standard. Prepare a series of chromium oxide standard solutions, determine the photometric value, and draw a standard working curve.
4.3.5.4 Calculation of results
According to the measured absorbance of the test solution, the corresponding content of lead oxide is found from the standard working curve, and the content of chromium trioxide in the sample is calculated according to the following formula:
Cr20% = w×100× 100
Wherein, m is the amount of chromium trioxide in the test solution obtained from the standard working curve, mg; W is the sample weight, mg.
4.3.6 Determination of phosphorus
4.3.6.1 Key points of the method
SJ/T 10461-93
After stirring and dissolving, the ammonium vanadium molybdate color developer is mixed with phosphorus yellow vanadium platinum heteropoly acid in nitric acid medium and quantified by spectrophotometry.
4.3.6.2 Reagents and solutions
Nitric acid;
b, perchloric acid;
c. Ammonium vanadate molybdate color developer,
Dissolve 10g of ammonium lead acid in 100ml of 60-70% water. If there is precipitation or confusion, it must be filtered before use. b0.8g of ammonium vanadate is dissolved in 5gml water, heated to dissolve at 50-60℃, cooled, and 50ml of (1+3) nitric acid is added. The color developer is slowly poured into b, stirring while adding, and then 18ml of nitric acid is added, transferred to a brown reagent bottle, and stored in a dark place for later use. d, phosphorus standard solution (phosphorus pentoxide ~ 50μg/ml) Weigh 0.9585g of the standard potassium dihydrogen phosphate reagent dried at 110-130℃, (KH,P0,) in a beaker, dissolve, transfer to a 500ml container bottle, and dilute to the scale with water. Shake the hook, draw 10ml of the solution into a 200ml volumetric flask, and dilute to the mark with water (containing 50μg/ml phosphorus pentoxide):
4.3.6.3 Analysis steps
a. Weigh 1-2 samples into a 100ml beaker, add 30ml of water and 5ml of nitric acid, heat to dissolve, evaporate until the salts are folded out, add 5ml of nitric acid, continue to dissolve by heating, and evaporate to near dryness. Cool, add 2ml nitric acid, appropriate amount of water, heat to dissolve salts, transfer to a 50ml volumetric flask after it is clear, add 5ml color developer, dilute to scale with water, shake well, leave for 10-30min, measure the absorbance at 420mm with the reagent blank as reference:
b, take 0, 1.3, 5.7, 9ml of phosphorus standard solution into a 50ml volumetric flask, add water to about 30ml, add 2ml of boiled nitric aldehyde and 5ml of color developer solution, dilute to scale with water, shake well. Leave for 10-30min, measure the absorbance at 420m at the same time as the sample solution, and draw a standard working curve. 4.3.6.4 Calculation of results
According to the measured absorbance of the test solution, the amount of phosphorus pentoxide in the test solution is found from the standard working curve, and the content of phosphorus pentoxide is calculated according to the following formula:
P20,%=
w×1000
Wherein: M--the amount of phosphorus pentoxide in the test solution found from the standard curve, mg W--the sample, g.
4.3.7 Determination of chlorine
4.3.7.1 Key points of the method
After the sample is dissolved, add ammonium ferric sulfate solution and mercuric thiouracil to dissolve, and quantify the trace chlorine in the sample by measuring the absorbance of the red complex formed by the sulfhydryl ion replaced by fluorine and iron. 4.3.7.2 Reagents and solutions
a, nitric acid (superior grade), (1+2):
b. Sulfuric acid (superior grade), (1 +1);
c, Ammonium ferric sulfate solution, 6%
SJ/T 1046193
Weigh 60g of ammonium ferric sulfate (superior grade) [Fe,(S0)(NH.)zSU4-24H,Oj and dissolve it in 1000ml of nitric acid (12), Mercuric thiocyanate ethanol solution, 0.3%
Weigh 1.5g of mercuric sulfhydryl [Hg(SCN)2] and dissolve it in 500ml of 95% ethanol; e. Chloroquine solution (5μg/ml)
Dry the standard sodium chloride at 500-600℃ for 4050min, put it in a cold room in a desiccator, accurately weigh 0.8240g and dissolve it in water, transfer it into a 1000ml volumetric flask and dilute to the scale. Then take 10ml of this solution into a 1000ml volumetric flask and dilute it to the mark with water. According to the hook, it is used as the chlorine standard solution.
4.3,7.3 Analysis steps
, weigh 1.0g of the sample into a 200ml beaker, add water, 15ml of nitric acid (1+2), heat to dissolve, drive out carbon dioxide, and make the solution volume about 45~50ml. Add 3ml of sulfuric acid (1+1) dropwise under hot water, slowly heat to a slight boil, keep warm for more than 4h, filter slowly with filter paper, wash with water 2~3 times, collect the filtrate and washing liquid in a 100ml volumetric flask, control the solution to about 70ml, add 10ml of ferric sulfate solution and 5ml of mercuric thiocyanate solution, shake well, keep mixing at room temperature for 10min, dilute with water to the mark, shake well. Use 2cm colorimetric III, reagent blank as reference, and measure the absorbance 2 at a wavelength of 460nm. Note: 1) The color development speed is related to temperature and should be prepared under the same conditions as the standard curve. 2) The coexistence of Bx, I, CN\ will interfere with the test. b. Pipette 0.10.20.30.40, 50ml of fluorine standard solution into a 100ml bottle, add water to about 70ml… The following is carried out according to the sample analysis step 4.3.7.3a. Determine the absorbance of the standard series solution and draw a standard working curve. 4.3.7.4 Result calculation
According to the measured absorbance of the test solution, find out its corresponding oxygen content from the standard working curve, and calculate the chlorine content in the sample according to the following formula:
C1% = wx1000 ×100
Where: M——the amount of chlorine in the test solution found from the standard working curve, Ⅱg; W is the sample weight, B.
4.3.8 Determination of cobalt oxide, nickel oxide and manganese dioxide 4.3.8.1 Key points of the method
After the sample is dissolved, drive out the carbon dioxide and measure the atomic absorbance of cobalt, nickel and manganese in the test solution in nitric acid medium with an atomic absorption spectrophotometer.
4.3.8.2 Reagents and solutions
a. Nitric acid 1+1;
b. Cobalt oxide (COO) standard solution (0.5mg/ml) Accurately weigh 0.3553g of metallic cobalt (more than 99.99%) in a 200ml beaker, add (1i1) nitric acid 50ml, dissolve at low temperature, add a small amount of water and boil. After cooling, transfer to a 1U00ml container, dilute to the scale with water and shake well. c. Nickel oxide (NiO) standard solution (1mg/ml) Accurately weigh 0.7860g of metallic nickel (99.99% or more) in a 200ml beaker, add 15ml of 1+1 nitric acid, dissolve at room temperature, add a small amount of water, boil, cool and transfer to a 1000ml volumetric flask, dilute to scale with water, and shake well. d. Manganese dioxide standard solution (1ng/ml)-9
SJ/T 10461-93
Accurately weigh 0.6319g of metallic manganese [99.99% or more, wash off the surface oxide layer with dilute sulphuric acid before weighing, wash with water to remove acid, dehydrate with ethanol, and dry) in a 200ml beaker, add 20ml of (1+1) nitric acid, dissolve at room temperature, boil, cool and transfer to a 1000ml volumetric flask. Dilute to scale with water and add 1ng/ml of nitric acid to remove acid. t. Cobalt, nickel, manganese mixed standard solution
Pipette 30ml of cobalt oxide standard solution, 50ml of nickel oxide standard solution, and 50ml of manganese dioxide standard solution respectively, into a 1000ml volumetric flask, dilute to scale with water, and spread evenly. f. Cobalt, nickel, manganese mixed standard solution series Accurately pipette 0.1, 2.3, 4, 5ml of cobalt, nickel, manganese mixed standard solution respectively into a 50ml volumetric flask, add (1+1) nitric acid 5mil each. Dilute to the mark with water, and shake well. A series of mixed standard solutions are formed, and their concentrations are shown in Table 5. Table 5 Series of cobalt, nickel, manganese mixed standard solutions
CO,Os(pg/ml)
Nio(jag/mal)
MrO(μg/ml)
Analysis elements
Analysis line
4.3.8.3 Analysis steps
Table 6 Determination conditions for cobalt, nickel and manganese
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Air-acetylene||t t||Air-acetylene
Air-acetylene
Flow rate (L/min)
Combustion-supporting gas
Combustible gas
Accurately weigh 5g of sample, put it in a 100ml beaker, add about 10ml of water, shake well, and drop 1:1 nitric acid solution to dissolve the sample. After the reaction is complete, add 5ml of 1:1 nitric acid, heat to a slight boil, and drive out carbon dioxide gas: after cooling, transfer to a 50ml volumetric flask, if there is any mixture, filter and dilute to the scale with water. According to the determination conditions in Table 6, determine the atomic absorbance of cobalt, nickel, and manganese simultaneously with the mixed standard solution series. Draw a standard working curve.
4.3.8.4 Result screening
According to the absorbance of each element in the test solution, find the concentration of the corresponding oxide from the standard working curve, and calculate the content of each oxide in the sample according to the following formula.
Wherein: MO—represents the oxide of cobalt, nickel or palladium: × 50
w × 1000
C--the concentration of the oxide (cobalt oxide or nickel oxide or manganese dioxide) found from the standard working curve, mg/ml;
W is the sample weight.g.
4.4 Determination of Adherent Moisture
4.4.1 Instrument
Infrared Moisture Analyzer.
Adjust and zero before each determination.
4.4.2 Determination Method
SJ/T 10461-93
4.4.2.1 After the sample is fully mixed, weigh 20g of the sample on the weighing dish of the moisture analyzer and spread the sample flat. 4.4.2.2 Adjust the indicator indicating the percentage of moisture to zero, and the pendulum needle indicating the weighing balance also indicates zero. Turn on the infrared lamp and heat the sample. Start with 3 minutes, keep the voltage at 100V, then reduce it to 60V until the pointer of the moisture content is stable. During the measurement, keep turning the indicating dial of the moisture content to keep the pendulum needle always aligned with the zero position. Record the reading at the static point of the pendulum needle. That is, the sample is attached to the moisture content.
4.4.2.3 Use a thermometer to indicate the temperature, which can usually be kept at around 100. 5 Inspection rules
5.1 Inspection classification
Strontium carbonate products should be inspected before delivery. If necessary, the purchaser can conduct a re-inspection at the factory. 5.2 Factory inspection
Factory inspection The quality inspection department of the production unit shall conduct a comprehensive inspection of strontium carbonate according to the technical requirements and inspection methods specified in this standard to ensure that each batch of products meets the requirements of this standard. A test sheet and a quality certificate shall be attached. The certificate shall indicate the production unit, product name, batch number, batch size, production date and this standard number. 5.3 Re-inspection by the purchaser
The purchaser shall conduct a re-inspection of each batch of strontium carbonate purchased in accordance with the provisions of this standard, and the inspection shall be conducted within one month from the date of receipt of the product.
5.4 Inspection batch and sampling rules
The factory inspection batch consists of silver carbonate produced in one process cycle, and each batch shall not be less than 60T. The total amount purchased by the purchaser is considered as one batch. Use a stainless steel sampler to randomly select 10 packaging units from each batch, and the total sampling amount in each packaging unit shall not be less than 2kg. Mix and divide them, take 0.5kg of them and seal them with double plastic bags, put a label between the two plastic bags, and indicate the product name, manufacturer, product number, production date and batch on the label as the inspection sample. The remaining samples for inspection are still packaged and stored for one month for re-inspection. 5.5 Judgment rules
In the test results, if a certain index does not meet the requirements of this standard, the sample should be doubled for re-testing. If the re-test result shows that the index still does not meet the requirements of this standard, the batch of silver carbonate is unqualified. If there is a dispute between the supply and demand parties, the national recognized inspection department shall arbitrate according to the standard. 6 Marking, packaging, transportation and storage
6.1 Carbonic acid is packaged in plastic bags for the inner layer and woven bags for the outer layer. Small packages are sewn by a bag sewing machine. If there are special requirements, they shall be agreed upon by the supply and demand parties.
6.2 For each batch of packaged products, the bag shall be printed with the manufacturer's name, product name, net weight, and a product certificate. The certificate shall indicate: manufacturer's name, product name, batch number, weight and this standard number. 6.3 Strontium carbonate should be stored in a dry and clean place. During transportation, attention should be paid to waterproofing and avoiding damage and contamination. — —1 Carbonic acid, the inner layer is plastic bag, the outer layer is woven bag, small package is sewn by bag sewing machine, if there are special requirements, it shall be agreed by both parties.
6.2 Each batch of packaged products shall be printed with the manufacturer's name, product name, net raw material, and product certificate, which shall indicate: manufacturer's name, product name, batch number, weight and this standard number. 6.3 Strontium carbonate should be stored in a dry and clean place. It should be waterproof and avoid damage and contamination during transportation. — —1 Carbonic acid, the inner layer is plastic bag, the outer layer is woven bag, small package is sewn by bag sewing machine, if there are special requirements, it shall be agreed by both parties.
6.2 Each batch of packaged products shall be printed with the manufacturer's name, product name, net raw material, and product certificate, which shall indicate: manufacturer's name, product name, batch number, weight and this standard number. 6.3 Strontium carbonate should be stored in a dry and clean place. It should be waterproof and avoid damage and contamination during transportation. — —
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