Atomic-absorption spectrophotometry of impurties in clay,feldspar,magnesite,calcite,dolomite,talc,quartz for electron ceramic raw materials
Some standard content:
Electronic Industry Standard of the People's Republic of China
SJ/T10632-10633-1995
Electronic Ceramic Raw Materials
Atomic-absorption spectrophotometry for electron ceramic raw materials1995-04-22Promulgated
1995-10-01Implemented
The Ministry of Electronics Industry of the People's Republic of ChinaPromulgated Electronic Industry Standard of the People's Republic of China
Abomic-ahsnrptfon spectrophotonetry ofInpurties in elay, feldspur, magnesite,calcite,dolomite, lale, quartz toreleclrua cermie raw materials mmterials1 Main content and scope of application
1. 1 Content
Su/T10632-1995
Generation 511853-18551
511857185981
This standard specifies the atomic absorption spectrophotometric measurement method for impurities in electronic ceramic raw materials such as clay, feldspar, talc, calcite, dolomite, talc and quartz.
1.2. Scope of application
This standard applies to the measurement of calcium, magnesium, iodine, ferrite and various oxides in electronic ceramic raw materials such as clay, feldspar, talc, calcite, dolomite, talc and quartz.
2 Methods
After the sample is treated with gaseous acid and self-acid, it is dissolved with a dissolving agent, and the selected radioactive agent is used to eliminate the interference of aluminum on calcium and magnesium, and the photometry is measured. The result is calculated according to the standard. 3 Reagents
Ammonia
Lithium hydroxide
Calcium carbonate
Magnesium oxide
Titanium oxide
Kaihua Zhong
36%, 1 +1
Commercial line:
High purity:
High purity;
Commercial pure.
Superior purity;
Superior purity;
Low purity;
-short:
Approved by the Ministry of Electronics Industry of the People's Republic of China on April 22, 1995 and implemented on October 1, 1995
4 Equipment and precision equipment
SJ/T10632-1995
Original receiving spectrophotometer wavelength 200~800nm, single and double resolution 2nm/mm.
b, folding balance numerator is 0.1rg. Weighing should be accurate to 0.2mg, range 200gt, high and short furnace 1000 or more
d. Oven 25r:
Capacity 100500,10 00ml
1. Beaker 100, 150, 200ml:
E, platinum;
Good hot plate:Www.bzxZ.net
i. Volumetric volume:
Wine lamp,
5 Preparation of standard solution
5.1 Preparation of unit standard storage solution
5.1. Yipu standard solution: 1/l
Accurately weigh calcium carbonate 1.7948z that has been burned in 1W for 2h, put it in 100ml of agar, moisten it with water, then add 30ml of 1+1 hydrochloric acid and heat it to dissolve, drive off carbon monoxide, cool to room temperature, transfer into a 1[MIml container, dilute to the scale, pack, and store in a dry plastic bottle.
5.1.2 Magnesium oxide standard solution: lims/nl weigh 1.000g of magnesium oxide that has been calcined at 900°C for 2h, put it in a 0ml beaker, add 20ml of 1+1 salt. After dissolving, cool to room temperature, transfer to a 1000ml measuring cup, dilute to the scale, and store in a 1000ml plastic bottle. 5.1.3 Iron oxide standard solution: 1mx/cl
Accurately weigh 1.000 of iron oxide that has been calcined at 110°C for 2h 0g, put it in a 2K1ml olefin beaker, add 1+1m salt, heat to dissolve, cool to room temperature, transfer to a 0ml volumetric flask and dilute to the scale, store in a container for later use,
5.1.4 Potassium oxide standard solution: Accurately weigh 1.5830g of potassium oxide that has been dried at 110°C for 2h, put it in a 150ml beaker, add 10m hydrochloric acid, dissolve it in a 1000ml volumetric flask, add 10m hydrochloric acid, weigh to dissolve, and store in a dry plastic bottle for use. 5.1.5 Sodium hydroxide standard solution: 1mg/ml
Accurately weigh 1.88.59% sodium hydroxide that has been oxidized at 110°C for 2h, put it in a 150ml flask, add water to dissolve it, transfer it to a 1000ml flask, add 1ml of salt, mix well, and store it in a dry bottle for later use. 5.2 Preparation of standard solution
Separately add 1m3/ml calcium carbonate, 100ml of potassium oxide, 1m3/ml of sodium ion, 25ml each of sodium oxide and 10ml of 1mg/ml magnesium oxide, and place them in a 500ml volumetric flask. Add 10ml of 111) pad, add water to the bottle, shake it until the mark, and you will get the standard solution containing calcium oxide, 1.2mz/ml potassium oxide, 0.05mg/ml sodium oxide and 0.2mg/ml magnesium oxide, and store it in a reagent bottle. 5.3 Preparation of standard solution series
Take 0, 1, 2, 3, 4, 5 ml of the mixed standard solution in 5.2 and place them in 1 ml bottles. Add 10 ml of 20% sodium chloride 1.5r (1:1). Dilute with 1% Benzoate and mix well to obtain a standard solution series containing calcium oxide, iron oxide, potassium 2+, sodium 2+ and 2-nitrogen. 6 Analytical steps
6.1 Weigh 0.5 ml of the sample which has been dried at 110°C for 2 hours. 1000g, put in platinum liquid, moisten with water, add 1ml of high total weight and 10l of sodium chlorate, put on an electric hot plate, let it dry, wash the platinum liquid with a little water, add 1-2m】perchloric acid, evaporate to 1-2ml of hydrogen aldehyde fume, add 10ml of 1+1 solution, add water until it is active, cool to room temperature, transfer to a 100ml volumetric flask, add 20% silver hydroxide 2.5l, dilute to the scale, probe about 16.2 with 0.5% sodium hydroxide and 5% salt, magnesium, drink, stool, and tin oxide liquid as the tracking record, and then Perform absorption spectrophotometry and measure the concentration. If the sample contains a large amount of ions, add appropriate amounts of chemical and salt to the above test solution to maintain the concentration of 5% and the concentration of oxidized ions at 1.5%. 6.3 Adjust the combustion equipment on the instrument as scheduled. Preheat the hollow cathode lamp for 20 minutes and then ignite the flame. After normal combustion, check the room air and flow rate. Spray the sample with water or a blank solution, and then use a standard bottle to spray the sample and the test solution. Read the corresponding concentration and repeat the measurement with the same sample. The instrument setting is shown in the table below. |tt||The allowable amount is large and detailed
Note: The hollow electrode is modified according to the factory's regulations. The calculation of the split result
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Fire good state
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By determining the average value of the standard deep absorption width and the standard liquid concentration series, draw the standard surface line, and check the concentration of the element to be measured by the line, and then calculate the percentage of each element in the sample: M=×Vx 10-0
Wherein:
The average percentage of oxidizing agent in the test element is 2100%
The average percentage of oxidizing agent in the sample liquid is 2100%
G——sample mass.g;
vThe volume of the sample is narrow, ral
Additional instructions:
This standard was drafted by the Standardization Research Institute of the Ministry of Industry and the Standardization Research Institute of the Ministry of Electronics Industry, and the original authors are Zheng Yu, Liu Chengyue, and Bao Ying.
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