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GB/T 4325.6-2013 English PDF (GBT4325.6-2013)

GB/T 4325.6-2013 English PDF (GBT4325.6-2013)

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GB/T 4325.6-2013: Methods for chemical analysis of molybdenum -- Part 6: Determination of arsenic content -- Atomic fluorescence spectrometry

This Part of GB/T 4325 specifies the method to determine arsenic content in molybdenum. This Part is applicable to the determination of arsenic content in molybdenum powder, molybdenum bar, molybdenum trioxide, ammonium molybdate. The determination range is 0.0002%~0.0050%.
GB/T 4325.6-2013
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 77.120.99
H 63
Replacing GB/T 4325.5-1984
Methods for chemical analysis of molybdenum - Part
6: Determination of arsenic content - Atomic
fluorescence spectrometry
ISSUED ON: MAY 09, 2013
IMPLEMENTED ON: FEBRUARY 01, 2014
Issued by: General Administration of Quality Supervision, Inspection and Quarantine;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 6
2 Method summary ... 6
3 Reagents ... 6
4 Instruments ... 7
5 Specimen ... 8
6 Analysis steps ... 8
7 Calculation of analysis result ... 9
8 Precision ... 9
9 Test report ... 10
Foreword
GB/T 4325 ?€?Methods for chemical analysis of molybdenum?€? consists of the following 26 parts:
- Part 1: Determination of lead content - Graphite furnace atomic absorption spectrometry;
- Part 2: Determination of cadmium content - Flame atomic absorption
spectrometry;
- Part 3: Determination of bismuth content - Atomic fluorescence
spectrometry;
- Part 4: Determination of tin content - Atomic fluorescence spectrometry; - Part 5: Determination of antimony content - Atomic fluorescence
spectrometry;
- Part 6: Determination of arsenic content - Atomic fluorescence spectrometry; - Part 7: Determination of iron content - 1,10-phenanthroline
spectrophotometry and inductively coupled plasma atomic emission
spectrometry;
- Part 8: Determination of cobalt content - 5-Cl-PADAB spectrophotometry and flame atomic absorption spectrometry;
- Part 9: Determination of nickel content - Dimethylglyoxime
spectrophotometry and flame atomic absorption spectrometry;
- Part 10: Determination of copper content - Flame atomic absorption
spectrometry;
- Part 11: Determination of aluminum content ?€? Chrome azurol S
spectrophotometry and inductively coupled plasma atomic emission
spectrometry;
- Part 12: Determination of silicon content - Inductively coupled plasma atomic emission spectrometry;
- Part 13: Determination of calcium content - Flame atomic absorption
spectrometry;
- Part 14: Determination of magnesium content - Flame atomic absorption spectrometry;
Methods for chemical analysis of molybdenum - Part
6: Determination of arsenic content - Atomic
fluorescence spectrometry
1 Scope
This Part of GB/T 4325 specifies the method to determine arsenic content in molybdenum.
This Part is applicable to the determination of arsenic content in molybdenum powder, molybdenum bar, molybdenum trioxide, ammonium molybdate. The
determination range is 0.0002%~0.0050%.
2 Method summary
The test material is decomposed with hydrogen peroxide. In thiourea-ascorbic acid-hydrochloric acid medium, use hydride generation-atomic fluorescence spectrometry to determine arsenic content. Within a certain range, the
fluorescence intensity is proportional to the content of the measured element. Adding molybdenum matrix can eliminate interference.
3 Reagents
Unless otherwise specified, the reagents used in this Part are guaranteed reagents; water used is grade two or above.
3.1 Sodium borohydride.
3.2 Sodium hydroxide.
3.3 Molybdenum matrix (wAs???0.00002%).
3.4 Arsenic trioxide (wAs2O3???99.99%).
3.5 Nitric acid (??=1.42g/mL).
3.6 Hydrochloric acid (??=1.19g/mL).
3.7 Sulfuric acid (??=1.84g/mL).
3.8 Hydrogen peroxide.
3.9 Sulfuric acid (1+1).
3.10 Sulfuric acid (1+4).
3.11 Sodium hydroxide solution (200g/L).
3.12 Thiourea-ascorbic acid solution: Weigh 10g of thiourea and 10g of ascorbic acid respectively to dissolve in 200mL of water. Mix well. Prepare when it is required.
3.13 Arsenic standard stock solution: Weigh 0.1320g of arsenic trioxide (3.4). Add 20mL of water, 0.2g of sodium hydroxide (3.2). Heat to dissolve. Use sulfuric acid (3.10) to neutralize to slightly acidic. Transfer into a 1000mL volumetric flask. Use water to dilute to the scale. 1mL of this solution contains 100??g of arsenic.
3.14 Arsenic standard solution: Pipette 1.00mL of arsenic standard stock solution (3.13) into a 100mL volumetric flask. Add 10mL of hydrochloric acid (3.6). Use water to dilute to the scale. Mix well. 1mL of this solution contains 1??g of arsenic.
3.15 Sodium borohydride solution: Weigh 1.5g of sodium borohydride (3.1). Add into 100mL of water that 1g of sodium hydroxide (3.2) is pre-dissolved. Shake well after dissolving completely. Prepare when it is required.
3.16 Hydrochloric acid (1+9).
3.17 Argon: the volume fraction is not less than 99.99%.
4 Instruments
Atomic fluorescence spectrometer, with arsenic special hollow cathode lamp. Under the best working conditions of the instrument, anyone who can reach the following indicators can be used.
- Detection limit: not more than 1??10-9g/mL;
- Precision: use 0.02??g/mL arsenic standard solution to measure
fluorescence intensity 10 times; its standard deviation does not exceed 5.0% of the fluorescence intensity;
- Linear of working curve: divide the working curve into five equal segments according to the concentration; the ratio of the difference in fluorescence intensity between the highest segment and the lowest segment shall be

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