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GB/T 4325.5-2013 PDF English

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GB/T 4325.5-2013: Methods for chemical analysis of molybdenum - Part 5: Determination of antimony content - Atomic fluorescence spectrometry
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GB/T 4325.5: Historical versions

Standard IDUSDBUY PDFDeliveryStandard Title (Description)Status
GB/T 4325.5-2013130 Add to Cart Auto, 9 seconds. Methods for chemical analysis of molybdenum - Part 5: Determination of antimony content - Atomic fluorescence spectrometry Valid
GB/T 4325.5-1984199 Add to Cart 2 days Methods for chemical analysis of molybdenum--The molybdenum blue photometric method for the determination of arsenic content Obsolete

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GB/T 4325.5-2013: Methods for chemical analysis of molybdenum - Part 5: Determination of antimony content - Atomic fluorescence spectrometry


---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT4325.5-2013
GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.120.99 H 63 Replacing GB/T 4325.4-1984 Methods for chemical analysis of molybdenum - Part 5: Determination of antimony 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 ... 7 6 Analysis steps ... 8 7 Calculation of analysis results ... 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 5: Determination of antimony content - Atomic fluorescence spectrometry

1 Scope

This Part of GB/T 4325 specifies the method to determine antimony content in molybdenum. This Part is applicable to the determination of antimony content in molybdenum powder, molybdenum bar, molybdenum trioxide, ammonium molybdate. The determination range is 0.0001%~0.0050%.

2 Method summary

The test material is decomposed with nitric acid and hydrochloric acid. In hydrochloric acid medium, use hydride generation-atomic fluorescence spectrometry to determine antimony 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 Nitric acid (ρ=1.42g/mL). 3.4 Hydrochloric acid (ρ=1.19g/mL). 3.5 Sulfuric acid (ρ=1.84g/mL). 3.6 Hydrochloric acid (1+9). 3.7 Ammonia (1+99).

6 Analysis steps

6.1 Test material Weigh the specimen according to Table 1, to the nearest of 0.0001g. 6.2 Number of determination Perform two independent determinations. Take the average value. 6.3 Blank test In the presence of the same molybdenum matrix, do a blank test with the test material. 6.4 Determination 6.4.1 Place the test material (6.1) in a 150mL beaker. Add a little water to wet. Add 15mL of hydrochloric acid (3.4), 5mL of nitric acid (3.3). Cover with watch glass. Heat and completely dissolve at low temperature. Boil to drive off nitrogen oxides. Remove to cool. Transfer to a 100mL volumetric flask. Use water to dilute to the scale. Mix well. 6.4.2 On the atomic fluorescence spectrometer, use hydrochloric acid (3.6) as carrier, sodium borohydride solution (3.12) as reducing agent, use antimony special hollow cathode lamp as excitation light source to measure the fluorescence intensity of the test material solution. Subtract the fluorescence intensity of the blank solution accompanying the test material. Check the corresponding antimony concentration from the working curve. 6.5 Drawing of working curve 6.5.1 Pipette the molybdenum matrix solution (3.11) equivalent to the amount of test material. Place in a series of 100mL volumetric flasks. Respectively add 0mL, 0.10mL, 0.50mL, 1.00mL, 2.00mL, 5.00mL of antimony standard solution (3.10). Add 10mL of hydrochloric acid (3.4). Use water to dilute to the scale. Mix well. 6.5.2 Under the same conditions as the measurement of test material solution, measure the fluorescence intensity of the series of standard solutions. Subtract the fluorescence intensity of the "zero" concentration in the series of standard ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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