Determination of multi-element contents in high purity graphite used for siliconmaterial. Inductively coupled plasma atomic emission spectrographic method
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This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by China Iron and Steel Industry Association.
This standard is under jurisdiction of the National Technical Committee on Iron and Steel of Standardization Administration of China (SAC/TC 183).
Determination of multi-element contents in high purity graphite used for silicon material - Inductively coupled plasma atomic emission spectrographic method
1 Scope
This standard specifies the method for determining the contents of aluminum, calcium, copper, iron, potassium, magnesium, sodium, phosphorus, arsenic, zinc, nickel, chromium and boron in high purity graphite products for polysilicon by inductively coupled plasma atomic emission spectrographic method.
This standard is applicable to the determination of aluminum, calcium, copper, iron, potassium, magnesium, sodium, phosphorus, arsenic, zinc, nickel, chromium and boron in high purity graphite products for polysilicon, with the range shown in Table 1.
Table 1 Determination range
Element Mass fraction/(μg/g) Element Mass fraction/(μg/g)
Aluminum 1.00~10.00 Phosphorus 0.10~5.00
Calcium 1.00~50.00 Arsenic 0.10~5.00
Copper 0.10~5.00 Zinc 0.10~5.00
Iron 1.00~10.00 Nickel 0.10~5.00
Potassium 0.10~5.00 Chromium 0.10~5.00
Magnesium 0.10~5.00 Boron 0.10~5.00
Sodium 0.10~5.00
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 6682-2008 Water for analytical laboratory use - Specification and test methods
GB/T 8170 Rules of rounding off for numerical values & expression and judgment of limiting values
3 Principle
Weigh a certain amount of specimen, put it in a muffle furnace, heat it from room temperature to 980~1,020℃ until it is completely incinerated. Dissolve the ash by chemical method, introduce the specimen solution into an inductively coupled plasma atomic emission spectrometer, and determine the content of each element in the specimen solution under the selected determination conditions.
4 Reagents
4.1 All test water shall meet the requirements for Class-I water as specified in GB/T 6682-2008.
4.2 Hydrochloric acid, with ρ of about 1.19g/mL, and the impurity content of each metal of lower than 100ng/L.
4.3 Hydrochloric acid, (1+1).
4.4 Single-element standard stock solutions: domestic or foreign certified standard samples which are traceable in terms of measurement size, and having a mass concentration of 1,000μg/mL.
4.5 Mixed standard solution: respectively transfer 1.00mL standard stock solutions (see 4.4) of boron, phosphorus, sodium, potassium, chromium, aluminum, calcium, copper, zinc, arsenic, magnesium, nickel and iron into a 100mL PFA volumetric flask, add 10mL hydrochloric acid (see 4.3), dilute with water to the scale, and then shake well. In this way the content of each element in this solution is 10μg/mL.
5 Instruments and apparatus
5.1 Inductively coupled plasma atomic emission spectrometer.
5.2 Electronic balance: with a sensitivity of 0.0001g.
5.3 Oven: with a working temperature of 105~110℃.
5.4 Muffle furnace: with a working temperature of 1,000±20℃, and a φ10~15mm round hole in the furnace door.
5.5 Electric heating plate: with a working temperature of 120℃.
5.6 Porcelain ark: with a specimen loading capacity of 5~10g; or platinum dish: with a volume of 50mL.
5.7 PFA volumetric flask: 50mL.
5.8 PTFE beaker: 50mL.
5.9 Bench drilling and milling machine.
6 Interference factors
6.1 Scrape off the surface layer of the specimen with a clean scraper, and then drill the specimen with a cemented carbide drill to avoid the pollution of specimen by surface stain.
6.2 The surface of the drill shall be cleaned with anhydrous ethanol, so as not to pollute the specimen.
6.3 The sample shall be spread on the porcelain ark to avoid flame during calcination, which will reduce the amount of specimen by blowing it way.
7 Specimens
Drill specimens with a cemented carbide drill, screen them by passing through 0.25mm standard sieve and dry them at 105~110℃ for 1.5h.
Foreword i
1 Scope
2 Normative references
3 Principle
4 Reagents
5 Instruments and apparatus
6 Interference factors
7 Specimens
8 Analytical procedures
9 Result calculation
10 Allowable error
11 Test report
