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SH/T 1499.5-1997 English PDF (SHT1499.5-1997)

SH/T 1499.5-1997 English PDF (SHT1499.5-1997)

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SH/T 1499.5-1997: Pure adipic acid. Determination of content of iron-2, 2?€?-Bipyridyl spectrophotometric method

This standard specifies the 2,2-bipyridine spectrophotometric method for the determination of iron content in pure adipic acid. This standard is applicable to the determination of iron content in pure adipic acid. AND the minimum determination concentration is 0.1 mg/kg.
SH/T 1499.5-1997
SH
PETROCHEMICAL INDUSTRY STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
ICS 71.080.40
G 15
Pure adipic acid ?€? Determination of content of iron ?€?
2, 2?€?-Bipyridyl spectrophotometric method
ISSUED ON. JULY 12, 1997
IMPLEMENTED ON. DECEMBER 01, 1997
Issued by. China Petrochemical Corporation
Table of contents
Foreword ... 3
1 Scope ... 4
2 Normative reference ... 4
3 Method summary ... 4
4 Reagents and solutions ... 5
5 Instruments and equipment ... 5
6 Sampling ... 5
7 Analytical procedures ... 5
8 Expression of analytical results ... 6
9 Precision... 6
10 Report ... 7
Foreword
This standard equivalently adopts the international advanced standards, uses the test methods of the 2, 2'-bipyridine spectrophotometric method as specified in clause 2.7 Determination of iron contents in SH/T 1499-92 after review, changes the number of standard samples for the purposes of working curve drawing from 12 to 7, AND determines the precision of the 95% confidence level using the mathematical statistics method.
This version was rewritten in accordance with the editing requirements of GB/T 1.1-1993, AND the chapter is fully supplemented and adjusted.
This standard shall, from the date of implementation, replace the clause 2.7 Determination of iron content in SH/T 1499-92.
This standard was proposed by Liaoyang Petrochemical Company.
This standard shall be under the jurisdiction of the National Chemical
Standardization Technical Committee Petrochemical Technical Subcommittee. This standard is responsibly drafted by Liaoyang Petrochemical Company
Quality Inspection Department.
The main drafters of this standard. Xu Yan, Guo Shurong, Wang Ze?€?an, Ying Yuzhi, Wen Rong.
This standard was first published on October 10, 1986, AND first confirmed on July 12, 1997.
Pure adipic acid ?€? Determination of content of iron ?€?
2, 2?€?-Bipyridyl spectrophotometric method
1 Scope
This standard specifies the 2,2'-bipyridine spectrophotometric method for the determination of iron content in pure adipic acid.
This standard is applicable to the determination of iron content in pure adipic acid. AND the minimum determination concentration is 0.1 mg/kg.
2 Normative reference
The provisions in following documents become the provisions of this Standard through reference in this Standard. The versions indicated at the time of publication of this standard are valid. All standards are subjected to revision, AND parties who reach an agreement based on this Standard are encouraged to study if the latest versions of these documents are applicable.
GB/T 601-88 Chemical reagent ?€? Preparations of standard volumetric
solutions
GB/T 602-88 Chemical reagent ?€? Preparations of standard solutions for
impurity (eqv ISO 6853-1.1982)
GB/T 6678-86 General principles for sampling chemical products
GB/T 6679-86 General rules for sampling of solid chemical products
GB/T 6682-92 Water for laboratory use; Specifications
SH/T 1499.4-1997 Pure adipic acid ?€? Determination of ash
3 Method summary
After the sample is subjected to ashing dissolution, the trivalent iron ions in the ash are reduced to divalent iron ions by hydroxylamine hydrochloride under acidic conditions, the divalent iron ions react with 2,2'-bipyridyl to form red complexes, the absorbance of which is determined at the wavelength 522nm, AND the iron content of the sample is calculated in accordance with the working curve.
mark; LET it stand for 10min. On the spectrophotometer, USE the 5cm
absorption pool at the wavelength 522nm to determine the absorbance of each solution using water as reference.
USE the iron content (mg) as the abscissa AND the net absorbance (solution absorbance deducted by blank solution absorbance) as the ordinate, to draw the working curve.
7.2 Determination of samples
In accordance with the requirements of SH/T 1499.4, ADD 10mL of
hydrochloric acid (4.1) into the platinum dish (or porcelain crucible) which had been subjected to ash content determination; EVAPORAE it dry in sand bath; REPEAT this operation for 2 times. In the hydrochloric acid evaporation process, it is required to shake the platinum dish frequently to make all the surfaces with ash are immersed in acid, to dissolve all the components of ash which can be dissolved in hydrochloric acid. Then ADD 10mL of hydrochloric acid solution (4.5); HEAT it on the sand bath and FILTER it; USE hydrochloric acid solution (4.5) to rinse it for three times, about 5mL every time; quantitively TRANSFER the filtrate and rinsing solution into a 100mL volumetric flask; AND the rest procedures follows the requirements of clause 7.1. And meanwhile CONDUCT one blank test (that is, without adding sample).
8 Expression of analytical results
8.1 Calculation
The iron content x (mg/kg) in the sample is calculated in accordance with the formula (1).
Where.
m1 ?€? The mass of iron as found from the working curve of the sample
solution net absorbance, mg;
m ?€? The mass of sample, g.
8.2 Expression of results
The arithmetic mean of the results of repeated measurements is taken as the result of the analysis, which shall be accurate to 0.1 mg/kg.
9 Precision
9.1 Repeatability

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