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GB/T 223.89-2019 PDF English

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GB/T 223.89-2019: Iron, steel and alloy - Determination of tellurium content - Hydride generation-atomic fluorescence spectrometric method
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GB/T 223.89-2019130 Add to Cart Auto, 9 seconds. Iron, steel and alloy - Determination of tellurium content - Hydride generation-atomic fluorescence spectrometric method Valid

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GB/T 223.89-2019: Iron, steel and alloy - Determination of tellurium content - Hydride generation-atomic fluorescence spectrometric method


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NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.080.01 H 11 Iron, steel and alloy - Determination of tellurium content - Hydride generation-atomic fluorescence spectrometric method ISSUED ON: AUGUST 30, 2019 IMPLEMENTED ON: JULY 01, 2020 Issued by: State Administration for Market Regulation; Standardization Administration of the People's Republic of China.

Table of Contents

Foreword ... 3 1 Scope ... 4 2 Normative references ... 4 3 Principle ... 5 4 Reagents ... 5 5 Instruments ... 6 6 Sample taking and preparation ... 7 7 Analysis steps ... 7 8 Result calculation ... 10 9 Precision ... 11 10 Test report... 11 Annex A (informative) Precision test related information ... 13 Iron, steel and alloy - Determination of tellurium content - Hydride generation-atomic fluorescence spectrometric method CAUTION - The personnel using this Part shall have hands-on experience in formal laboratory work. This Part does not address all possible safety issues. It is the responsibility of users to take appropriate safety and health measures and to ensure compliance with the conditions set by the relevant national regulations.

1 Scope

This Part of GB/T 223 specifies a method for the determination of tellurium content by hydride generation-atomic fluorescence spectrometric method. This Part applies to the determination of tellurium content in iron, steel and alloy. The determination range is 0.00001 % ~ 0.005 % of mass fraction.

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 6379.1 Accuracy (trueness and precision) of measurement methods and results - Part 1: General principles and definitions GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method GB/T 6682 Water for analytical laboratory use - Specification and test methods GB/T 20066 Steel and iron - Sampling and preparation of samples for the determination of chemical composition WEIGH 10 g of potassium borohydride; DISSOLVE in potassium hydroxide solution (5 g/L) and DILUTE to 500 mL. Prepare before use. 4.12 Tellurium standard solution 4.12.1 Tellurium standard stock solution, 100 μg/mL WEIGH 0.1000 g of pure tellurium (the mass fraction of tellurium is not less than 99.99 %); PLACE in a 150 mL beaker; ADD 10 mL of nitric acid (see 4.6); COVER the surface dish; HEAT to complete dissolution at low temperature; TRANSFER to a 1000 mL volumetric flask; DILUTE to the mark with water; MIX well. 1 mL of this solution contains 100 μg of tellurium. 4.12.2 Tellurium standard solution A, 10.0 μg/mL PIPETTE 10.0 mL of tellurium standard stock solution (see 4.12.1); PLACE in a 100 mL volumetric flask; DILUTE to the mark with hydrochloric acid (1+9); MIX well. 1 mL of this solution contains 10.0 μg of tellurium. 4.12.3 Tellurium standard solution B, 1.0 μg/mL PIPETTE 10.0 mL of tellurium standard solution A (see 4.12.2); PLACE in a 100 mL volumetric flask; DILUTE to the mark with hydrochloric acid (1+9); MIX well. 1 mL of this solution contains 1.0 μg of tellurium. 4.12.4 Tellurium standard solution C, 0.10 μg/mL, prepare before use PIPETTE 10.0 mL of tellurium standard solution B (see 4.12.3); PLACE in a 100 mL volumetric flask; DILUTE to the mark with hydrochloric acid (1+9); MIX well. 1 mL of this solution contains 0.10 μg of tellurium.

5 Instruments

Non-dispersive atomic fluorescence spectrometer, fitted with hydride generator and special tellurium hollow cathode lamp. After optimization, the non-dispersive atomic fluorescence spectrometer used shall achieve the following indicators: a) Short-term precision: Measure the fluorescence intensity of the tellurium 5 %, precipitate will occur at the bottom of the beaker. The precipitate may be crushed with a glass rod and then ammonium fluoride solution (see 4.9) is added. Table 2 -- Acid used to dissolve different types of samples Sample type Amount of hydrochloric acid and nitric acid used Medium and low alloy steels of which the mass fraction of pure iron, pure nickel and chromium is less than 5 % Add 5 mL of nitric acid (see 4.6) to decompose the sample, and then add 7.5 mL of hydrochloric acid (see 4.3) Stainless steel 10 mL of hydrochloric acid, nitric acid mixed acid (see 4.7) Superalloy 10 mL of hydrochloric acid, nitric acid mixed acid (see 4.8) 7.3.2 Treatment of test solution 7.3.2.1 Mass fraction of tellurium is not greater than 0.0005 % TRANSFER the test solution (see 7.3.1) to a 50 mL volumetric flask; ADD 15 mL of hydrochloric acid (see 4.3) and 15 mL of citric acid solution (see 4.10); COOL to room temperature; DILUTE to the mark with water; MIX well; PLACE for 40 min for determination. 7.3.2.2 Mass fraction of tellurium is greater than 0.0005 % TRANSFER the test solution (see 7.3.1) to a 50 mL volumetric flask; DILUTE to the mark with water; MIX well. PIPETTE 5.0 mL of test solution; PLACE in a 50 mL volumetric flask; ADD 24 mL of hydrochloric acid (see 4.3), 2.5 mL of ammonium fluoride solution (see 4.9), 15 mL of citric acid solution (see 4.10); COOL to room temperature; DILUTE with water to the mark; MIX well; PLACE for 40 min for determination. 7.3.3 Measurement of atomic fluorescence intensity START UP; SET the lamp current and negative high voltage; PREHEAT at least 20 min before measurement; OPTIMIZE the instrument according to the instrument specifications. PREPARE potassium borohydride solution (see 4.12) and test solution (see 7.3.2.1 or see 7.3.2.2); USE hydrochloric acid (see 4.4) as the carrier; MEASURE the atomic fluorescence intensity of tellurium in the test solution according to the set procedure. The atomic fluorescence intensity of tellurium in the test solution minus the atomic fluorescence intensity of tellurium in the blank solution of the sample is the net atomic fluorescence intensity. 7.4 Plotting of calibration curve 7.4.1 Mass fraction of tellurium is not greater than 0.0005 % micrograms per milliliter (μg/mL); f - the diluting factor; V - the volume of the test solution to be tested, in milliliters (mL); m - the value of the sample mass, in grams (g). The analysis results retain 2 significant figures.

9 Precision

The precision of this Part is determined by a joint test of 9 levels of tellurium in 11 laboratories. Each level is tested twice in each laboratory under the repeatability conditions specified in GB/T 6379.1. The samples used and the precision test results are listed in Annex A. The test results reported by each laboratory are statistically analyzed according to GB/T 6379.2. The correlation between the obtained tellurium content and the repeatability limit r and the reproducibility limit R is shown in Table 5. Table 5 -- Repeatability and reproducibility of tellurium Element Range/% Repeatability limit r Reproducibility limit R Tellurium 0.00001 ~ 0.005 m in the formulas is the average value of the two measured values, expressed in % (mass fraction). The repeatability limit r and the reproducibility limit R are obtained according to the formulas given in Table 5. Under repeatability conditions, the absolute difference between the two independent test results is not greater than the repeatability limit r, on the premise that the repeatability limit r is greater than 5 %. Under reproducibility conditions, the absolute difference between the two independent test results is not greater than the reproducibility limit R, on the premise that the reproducibility limit R is greater than 5 %.

10 Test report

The test report shall include the following: a) all materials required to identify samples, laboratories and test dates; ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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