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GB/T 1515-2002Manganese ores--Determination of phosphorus content--Phosphomolybdenum blue spectrophotometric method (English PDF)

锰矿石磷含量的测定磷钼蓝分光光度法

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Issued by

General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China

Level / Type

National · Recommended

Issue date

September 11, 2002

Implementation date

April 1, 2003

Scope

GB/T 1515-2002 is the English-translated version of 锰矿石磷含量的测定磷钼蓝分光光度法.

GB/T 1515-2002 is the Chinese national standard on manganese ores--determination of phosphorus content--phosphomolybdenum blue spectrophotometric method, in the field of mining and minerals. The /T suffix marks it as a recommended standard: it is not compulsory by itself, but it becomes binding as soon as a contract, a tender or a customer specification calls it up - which in practice is how most foreign buyers meet it. It was issued on 11 September 2002 by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, and has been in force since 1 April 2003. Classification: ICS 73.060.20, CCS D32. This page is published from the official record of the standard held by the Chinese standards administration: the identification, the dates, the classification and the issuing body are taken from there. The clause text, the tables and the numeric limits are in the document itself, which is delivered complete in English translation.

Document preview — GB/T 1515-2002

National Standard of the People's Republic of China

ICS: 73.060.20
Classification: D32

Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China

1 Scope
2 Normative references
3 Principles
4 Reagents and materials
4.2 Hydrofluoric acid (rho
4.3 Hydrochloric acid (rho
4.10 Phosphorus standard solution
5 Instruments
6 Sampling and specimen preparation...
7 Analytical procedures...
7.3.2 Color development and measurement
7.3.2.1 Divide the filtrate into a 50 mL volumetric flask, according to Table 2. Add
7.3.3 Plotting the calibration curve
8 Result calculation...
9 Tolerance...

1 Scope

This Part specifies the principles, reagents and materials, instruments, sampling and specimen preparation, analytical procedures, calculation of results, etc., for the determination of phosphorus content, through the phosphomolybdenum blue spectrophotometric method. This Part applies to the determination of phosphorus content in manganese ore and aluminum concentrate; the determination range (mass fraction) is: 0.010% ~ 1.00%.

2 Normative references

The provisions in following documents become the provisions of this Part through reference in this Part. For the dated references, the subsequent amendments (excluding corrections) or revisions do not apply to this Part; however, parties who reach an agreement based on this Part are encouraged to study if the latest versions of these documents are applicable. For undated references, the latest edition of the referenced document applies.

GB/T 2011 Method of sampling and sample preparation of manganese ores in bulk

GB/T 14949.8-1994 Manganese ores - Determination of hygroscopic moisture content in analytical samples

3 Principles

The sample is decomposed by hydrochloric acid, hydrofluoric acid, sulfuric acid; the residue is melted; the pentavalent arsenic is reduced by sodium carbonate to trivalent arsenic. Phosphorus (V) and ammonium molybdate form molybdophosphoric heteropoly acid. After reduced by ascorbic acid, it forms phosphomolybdenum blue. Then the absorbance is measured, the phosphorus content is calculated.

4 Reagents and materials

Unless otherwise stated, only reagents confirmed to be analytically pure and distilled water or water of equivalent purity are used in the analysis.

4.1 Anhydrous sodium carbonate.

4.3 Hydrochloric acid (rho

4.4 Hydrochloric acid (1 + 50).

4.5 Sulfuric acid (1 + 1).

4.6 Sulfuric acid (1 + 3).

4.7 Potassium iodide solution (200 g/L).

4.8 Ascorbic acid solution (10 g/L), which is prepared at the time of use.

4.9 Ammonium molybdate solution (40 g/L).

4.10 Phosphorus standard solution

4.10.1 Weigh 0.4394 g of the reference potassium dihydrogen phosphate, that was pre-dried at 105 °C ~ 110 °C for 2 hours AND cooled to room temperature in a desiccator. Dissolve it in water. Transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well. 1 mL of this solution contains 100 µg of phosphorus.

4.10.2 Pipette 100.00 mL of phosphorus standard solution (4.10.1), into a 1000 mL volumetric flask. Use water to dilute it the mark. Mix well. 1 mL of this solution contains 10 µg of phosphorus.

5 Instruments

The usual laboratory instruments are used in the analysis. water to wash the crucible. Add

1.5 mL of sulfuric acid (4.5). Concentrate the solution to 10 mL ~ 15 mL.

7.3.1.3 Add 5 mL of potassium iodide solution (4.7). Heat it to a slight boil. After cooling, transfer the solution into a 100 mL volumetric flask. Use water to dilute it to the mark. Mix well. Use fast filter paper to make dry-filtration (the filtrate should not be placed for a long time, to prevent trivalent arsenic from being re- oxidized to pentavalent arsenic).

7 Analytical procedures...

7.3.2.1 Divide the filtrate into a 50 mL volumetric flask, according to Table 2. Add

5.5 mL of sulfuric acid (4.6). Add 5 mL of ascorbic acid solution (4.8). Mix well. Add water along the bottle wall, to about 40 mL. Add

4.0 mL of ammonium molybdate solution (4.9), whilst shaking it. Use water to rinse the bottle neck. Mix well. Heat in a boiling water bath, for 5 min. Remove it. Use running water to cool it to room temperature. Use water to dilute it to the mark. Mix well. Put in a spectrophotometer. Use a 1 cm absorbing dish, to measure the absorbance. Find out the corresponding amount of phosphorus from the calibration curve.

7.3.2.2 Selection of measurement wavelength: When the phosphorus content (mass fraction) is <= 0.04%, use 825 nm; when the phosphorus content (mass fraction) > 0.04%, use 700 nm.

7.3.3 Plotting the calibration curve

7.3.3.1 Pipette 0 mL,

10.00 mL of phosphorus standard solution (4.10.2), respectively, into a group of 50 mL volumetric flasks. Add

6.5 mL of sulfuric acid (4.6). Then carry out color development, according to 7.3.2.1, from "Add 5 mL of ascorbic acid solution". Measure the absorbance at 700 nm AND draw a calibration curve.

7.3.3.2 Pipette 0 mL,

0.50 mL,

4.00 mL of phosphorus standard solution (4.10.2), respectively, into a group of 50 mL volumetric flasks. Add

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 12 pages — is available in the English PDF.

Referenced standards

Normative references

GB/T 2011 · GB/T 14949.8-1994

Similar standards

GB/T 1506-2016|GB/T 10322.8-2009|GB/T 13241-2017|GB/T 14352.12-2010|GB/T 14352.16-2010

Editions of GB/T 1515

Edition	Title	Revision	Status
GB/T 1515-2002	Manganese ores--Determination of phosphorus content--Phosphomolybdenum blue spectrophotometric method	current edition	Current
GB/T 1515-1979	Method for determination of phosphorus content in manganese ores	previous edition	Superseded

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