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SH/T 1499.4-2016 English PDF (SHT1499.4-2016)

SH/T 1499.4-2016 English PDF (SHT1499.4-2016)

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SH/T 1499.4-2016: Pure adipic acid - Determination of content of ash

This Part specifies the gravimetric method for the determination of ash content in pure adipic acid. This Part applies to the determination of adipic acid with the ash content of not less than 1 mg/kg.
SH/T 1499.4-2016
SH
PETROCHEMICAL INDUSTRY STANDARD
OF THE PEOPLE REPUBLIC OF CHINA
ICS 71.080.40
G 17
Filing No.. 55638-2016
Replacing SH/T 1499.4-1997
Pure adipic acid -
Determination of content of ash
ISSUED ON. JULY 11, 2016
IMPLEMENTED ON. JANUARY 1, 2017
Issued by. Ministry of Industry and Information Technology of the People?€? Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Method summary ... 5
4 Reagents and materials ... 5
5 Instruments and equipment ... 6
6 Sampling ... 6
7 Analysis steps ... 6
8 Expression of analysis results ... 7
9 Precision ... 7
10 Report ... 8
Foreword
SH/T 1499 ?€?Pure adipic acid?€? is divided into the following parts.
- Part 1. Specification;
- Part 2. Determination of content - Titrimetric method;
- Part 3. Determination of chroma of ammonia solution - Spectrophotometric method; - Part 4. Determination of content of ash;
- Part 5. Determination of content of iron - 2, 2?€?-Bipyridyl spectrophotometric method; - Part 6. Determination of content of iron - Simple method;
- Part 7. Determination of content of nitric acid - Spectrophotometric method; - Part 8. Determination of content of oxidizable compounds -Titrimetric method; - Part 9. Measurement of melt colour (in Pt-Co scale);
- Part 10. Determination of content of moisture - Thermogravimetric method. This Part is Part 4 of SH/T 1499.
This Part is drafted according to the rules given in ISO/IEC 1.1-2009.
This Part replaces SH/T 1499.4-1997 ?€?Pure adipic acid - Determination of content of ash?€?.
Compared with SH/T 1499.4-1997, the main changes of this Part are as follows. - MODIFY the standard name;
- ADD detection limits for the method (see Clause 1 of this Part);
- CHANGE the balance?€?s scale division value from ?€?0.1 mg?€? to ?€?0.01 mg?€?; ADD the requirements for the balance (see 5.1 of this Part, 5.1 of 1997 edition); - CHANGE the amount of the weighed sample from ?€?100 g?€? to ?€?100 g or 200 g?€? (see 7.2 of this Part, Clause 7 of 1997 edition);
- CHANGE the fractional digit of the result from ?€?1 mg/kg?€? to ?€?0.1 mg/kg?€? (see 8.2 of this Part, Clause 9 of 1997 edition);
- REDEFINE the reproducibility of the method and add the reproducibility (see 9.1 Pure adipic acid - Determination of content of ash
WARNING. This Standard is not intended to describe all safety issues related to its use. It is the responsibility of the user to take appropriate safety and health measures to ensure compliance with the relevant national regulations.
1 Scope
This Part specifies the gravimetric method for the determination of ash content in pure adipic acid.
This Part applies to the determination of adipic acid with the ash content of not less than 1 mg/kg.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the dated edition cited applies. For undated references, the latest edition of the referenced document (including all amendments) applies.
GB/T 6678 General principles for sampling chemical products
GB/T 6679 General rules for sampling of solid chemical products
GB/T 6682 Water for laboratory use - Specifications
3 Method summary
IGNITE the sample in a platinum crucible or porcelain crucible, BURN the combustion residue into ash at a (600 ?? 50) ??C muffle furnace, and then COOL and WEIGH. 4 Reagents and materials
Unless otherwise stated, all reagents are of analytical grade and the water used shall comply with the grade three water specifications specified in GB/T 6682. 4.1 Hydrochloric acid solution (1 + 4).
7.2 Sample measurement
USE a balance (5.2) to weigh the sample, ACCURATE to 0.01 mg. WEIGH (100 ?? 0.5) g of sample when the ash content is more than 2 mg/kg. When the ash content is not more than 2 mg/kg, WEIGH (200 ?? 0.5) g of sample. PLACE the sample into the constant-weight crucible; PLACE the crucible on the mud triangle; HEAT the sample with alcohol torch from the bottom and around until the sample is all melted, and then LIT the sample, REMOVE the heater, LET the sample natural burns until extinguishes. NOTE. If 200 g sample is weighed, it will be processed twice.
PLACE the crucible in a (600 ?? 50) ??C muffle furnace; REMOVE after burning for 30 min; PLACE in a dryer to cool for 30 min; REMOVE; USE a balance (5.2) to weigh (accurate to 0.01 mg). REPEAT the above burning, cooling and weighing process until the difference between the two weighing is less than 0.05 mg, that is the constant weight.
8 Expression of analysis results
8.1 Calculation
The ash content of the sample ??, in mg/kg, is calculated according to formula (1). ?? ??? ????????? ??? ???????????? ???10??? ... (1)
where.
m1 - the mass of the empty crucible, in grams (g);
m2 - the mass of the ash content and the empty crucible, in grams (g);
m - the mass of the sample, in grams (g);
8.2 Expression of results
The arithmetic mean of the results of two repeated measurements is taken as the analysis result, accurate to 0.1 mg/kg.
9 Precision
9.1 Repeatability
The absolute difference of the test results of two independent measurements independently carried out in the same laboratory, by the same operator, using the same

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