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Steel slag - Determination of fluoride content and chloride content - Ion chromatography
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GB/T 38216.2-2019: PDF in English (GBT 38216.2-2019) GB/T 38216.2-2019
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 77.140.99
H 34
Steel slag - Determination of fluoride content and
chloride content - Ion chromatography
ISSUED ON: OCTOBER 18, 2019
IMPLEMENTED ON: FEBRUARY 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 and materials ... 5
5 Instruments and equipment... 6
6 Sample preparation ... 7
7 Test steps ... 7
8 Calculation of test results ... 8
9 Precision ... 9
10 Test report ... 9
Annex A (normative) Flow chart of specimen analysis result acceptance
procedure ... 11
Annex B (informative) Experimental raw data ... 12
Steel slag - Determination of fluoride content and
chloride content - Ion chromatography
WARNING - Personnel using this Part shall have formal laboratory work
experience. This Part does not point out all possible security issues. The
user is responsible for taking appropriate safety and health measures and
ensuring compliance with the conditions stipulated by relevant national
laws and regulations.
1 Scope
This Part of GB/T 38216 specifies the method to determine the content of
fluorine and chlorine in steel slag by ion chromatography.
This Part is applicable to the determination of fluorine and chlorine content in
steel slag. Determination range (mass fraction): 0.05%~2.0% for fluorine,
0.005%~0.1% for chlorine.
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 2007.2, General rules for the sampling and sample preparation of
minerals in bulk-Manual method of sample preparation
GB/T 6682, Water for analytical laboratory use - Specification and test
methods
GB/T 8170, Rules of rounding off for numerical values & expression and
judgement of limiting values
GB/T 12806, Laboratory glassware - One-mark volumetric flasks
GB/T 12807, Laboratory glassware - Graduated pipettes
GB/T 12808, Laboratory glassware - One-mark pipettes
GB/T 36240-2018, Ion chromatographs
3 Principle
The specimen is decomposed by sulfuric acid. Fluorine and chlorine escape
with water vapor and separate from the sample. It is absorbed by absorption
liquid. Use ion chromatography to determine. Qualitatively determine fluorine
and chlorine by the peak time. Use the standard curve to quantitatively
determine.
4 Reagents and materials
Unless otherwise specified, the reagents used are guaranteed reagents, and
the experimental water is grade one water specified in GB/T 6682.
4.1 Sodium hydroxide.
4.2 Sodium fluoride, the reference substance.
4.3 Sodium chloride, the reference substance.
4.4 Concentrated sulfuric acid, ρ=1.84g/mL.
4.5 Sulfuric acid solution (2+1): Measure 200mL of concentrated sulfuric acid
(see 4.4) and slowly pour into 100mL of water. Mix well.
4.6 Sodium hydroxide solution c(NaOH)=0.2mol/L: Weigh 8.0g of sodium
hydroxide (see 4.1) and dissolve it in 1000mL of water.
4.7 Fluorine standard stock solution: Accurately weigh 2.2110g of standard
sodium fluoride that has been dried at 105°C±2°C for 2h (see 4.2). Use water
to dissolve. Transfer to a 1000mL volumetric flask. Use water to dilute to the
scale mark. Mix well. Transfer to a dry plastic bottle for storage. 1mL of this
solution contains 1000μg of fluorine.
4.8 Chlorine standard stock solution: Accurately weigh 1.6485g of reference
sodium chloride that has been burned to constant weight at 500°C~600°C (see
4.3). Dissolve in water. Transfer to a 1000mL volumetric flask. Use water to
dilute to the scale mark. Shake well. 1mL of this solution contains 1000μg of
chlorine.
4.9 Fluorine and chlorine mixed standard solution: Accurately pipette 5.00mL of
fluorine standard storage solution and chlorine standard storage solution
respectively (see 4.7 and 4.8) into a 50mL volumetric flask. Use water to dilute
to the scale mark. 1mL of this solution contains 100.0μg of fluorine or chlorine
respectively.
5.8 Glassware: All glassware must be soaked in 2mol/L sodium hydroxide
solution and water for 4h before use. Then use water to rinse 3~5 times. Let dry
and set aside.
5.9 The volumetric flask shall meet the requirements of GB/T 12806. The
pipette shall meet the requirements of GB/T 12807 and GB/T 12808.
6 Sample preparation
Prepare the specimen according to the method in GB/T 2007.2. The particle
size of the specimen is not greater than 0.080mm. Place the sieved specimen
in an oven (see 5.1) at 105°C±2°C for 1h. Take it out. Place it in a desiccator to
cool to room temperature for future use.
7 Test steps
7.1 Specimen amount
Weigh 0.5g of specimen, to the nearest of 0.0001g.
7.2 Number of determinations
For the same specimen, conduct at least two independent determinations.
7.3 Blank test
Do a blank test with the specimen.
7.4 Chromatographic analysis conditions
Debug the parameters such as chromatographic column temperature, elution
speed, suppression current, injection volume. Set aside for future use.
7.5 Determination
7.5.1 Take an appropriate amount of water and place it in the distillation flask of
the steam distillation device (see 5.4). Heat to make water boil, for future use.
7.5.2 Pipette 10mL of sodium hydroxide solution (see 4.6) into a 100mL
receiving bottle as the receiving solution, for future use.
7.5.3 Place the test material (see 7.1) in a three-necked round bottom flask.
Add 60mL of sulfuric acid solution (see 4.5). Use water to clean the mouth of
the bottle. Put in a few glass beads. Connect steam distillation device for
distillation. Heating makes the temperature of the solution in the three-neck
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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