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SH/T 1499.10-2012

Chinese Standard: 'SH/T 1499.10-2012'
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Detail Information of SH/T 1499.10-2012; SH/T1499.10-2012
Description (Translated English): Pure adipic acid. Part 10: Determination of content of moisture. Thermogravimetric method
Sector / Industry: Petrochemical Industry Standard (Recommended)
Classification of Chinese Standard: G17
Classification of International Standard: 71.080.40
Quoted Standard: GB/T 6678; GB/T 6679; GB/T 8170; GB/T 6283
Drafting Organization: China National Petroleum Corporation Liaoyang Petrochemical Company olefins plant
Administrative Organization: National Petrochemical Standardization Technical Committee Technical Committee
Regulation (derived from): Ministry of Industry and Information Technology Bulletin 2012 No. 20; industry standard filing Notice 2012 No. 8 (No. 152 overall)
Summary: This standard specifies the pyrolysis fine adipic moisture content determination. This standard applies to the determination of moisture content of adipic acid fine measuring range (0. 050 to 0. 300)% (mass fraction).

SH/T 1499.10-2012
SH
PETROCHEMICAL INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 71.080.40
G 17
Filing No.. 36918-2012
Pure adipic acid - Determination of content
of moisture - Thermogravimetric method
精己二酸 第 10部分. 水分含量的测定 热失重法
ISSUED ON. MAY 24, 2012
IMPLEMENTED ON. NOVEMBER 1, 2012
Issued by. Ministry of Industry and Information Technology of the People’
Republic of China
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Method summary ... 4
4 Instruments ... 4
5 Sampling ... 5
6 Analysis steps ... 5
7 Expression of results ... 6
8 Repeatability ... 6
9 Report ... 6
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 10 of SH/T 1499.
This Part is drafted according to the rules given in GB/T 1.1-2009.
This Part is proposed by China Petroleum & Chemical Corporation.
This Part is under the jurisdiction of Subcommittee on Petrochemistry of National
Technical Committee on Chemical of Standardization Administration of China (SAC/TC
63/SC 4).
Drafting organization of this Part. Liaoning Petrochemical Company of PetroChina Co.,
Ltd.
Main drafters of this Part. Zheng Limei, Zhang Yuanli,Su Changzhi, Wang Hongjie,
Zhang Peng, Han Zhijie, Wang Qun.
This is the first issue of this Part.
Pure adipic acid - Determination of content
of moisture - Thermogravimetric method
1 Scope
This Part specifies the thermogravimetric method for the determination of moisture
content in pure adipic acid.
This Part applies to the determination of the moisture content in pure adipic acid, the
determination range is (0.050 ~ 0.300) % (mass fraction).
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 8170 Rules of rounding off for numerical values & expression and judgement
of limiting values
GB/T 6283 Chemical products - Determination of water - Karl Fischer method
(general method)
3 Method summary
USE infrared moisture meter to heat and dry the pure adipic acid, to evaporate the
moisture. According to the mass change of the pure adipic acid sample before and
after evaporation of moisture, obtain the moisture content of pure adipic acid.
4 Instruments
4.1 Infrared moisture meter. capable of measuring the moisture content within the
range of (0.050 ~ 0.300) % (mass fraction); the display accuracy. 0.001 % (mass
fraction); equipped with automatic heating control system; equipped with automatic

SH/T 1499.10-2012
Pure adipic acid.Part 10. Determination of content of moisture.Thermogravimetric method
ICS 71.080.40
G 15
Record number. 36918-2012
SH
People 's Republic of China petrochemical industry standards
Pure adipic acid
Part 10. Determination of moisture content - Thermal weight loss method
Pure adipic acid-
Part 10. Determination of content of moisture-Thermogravimetric method
2012-05-24 release
2012-11-01 implementation
Issued by the Ministry of Industry and Information Technology of the People 's Republic of China
Preface
SH/T 1499 "refined adipic acid" is divided into the following parts.
- Part 1. Specifications;
- Part 2. Determination of content - Titration;
- Part 3. Determination of chroma of ammonia solution - Spectrophotometric method;
- Part 4. Determination of ash;
- Part 5. Determination of iron content 2,2 '- bipyridyl spectrophotometric method;
- Part 6. Fast method for the determination of iron content;
- Part 7. Determination of nitric acid content - Spectrophotometric method;
- Part 8. Determination of oxidizable content - Titration;
- Part 9. Determination of the color of the melt;
- Part 10. Determination of moisture content - Thermal weight loss method;
This section is part 10 of SH/T 1499.
This part is based on the rules given in ISO /IEC 1.1-2009.
This part is proposed by China Petroleum & Chemical Corporation.
This section is under the jurisdiction of the National Chemical Standard Technical Committee Petrochemical Subcommittee (SAC/TC63/SC4).
This part of the main drafters. Zheng Limei, Zhang Yuanli, Su Changzhi, Wang Hongjie, Zhang Peng, Han Zhijie, Wang Qun.
This part is released for the first time.
Crude adipic acid
Part 10. Determination of moisture content - Thermal weight loss method
1 Scope
This section specifies the thermogravimetric method for the determination of the adipic acid moisture content.
This part is applicable to the determination of the moisture content of pure adipic acid, the determination range is (0.050-0.300)% (mass fraction).
2 normative reference documents
The following documents are indispensable for the application of this document. For dated references, only the date of the date is appropriate
For use in this document. For undated references, the latest edition (including all modifications) applies to this document.
General rules for sampling of chemical products GB/T
General rules for sampling of solid chemical products GB/T
Representation and Judgment of Numeric Ratification Rule and Limit Value of GB/T 8170
GB/T 6283 Determination of moisture content in chemical products Karl Fischer method (general method)
3 method summary
The adipic acid is heated and dried by an infrared moisture meter to evaporate the water. According to the water before and after evaporation
The acidity of the diacid sample changes the moisture content of the adipic acid.
4 instruments
4.1 Infrared Moisture Analyzer. Can measure (0.050-0.300)% (mass fraction) of the water content, display accuracy. 0.001%
Volume fraction); equipped with automatic heating control system; equipped with automatic weighing system, the minimum scale value of 0.1 mg, according to the sample lost
The rate of change in the quality of the water process, that is, the slope to automatically determine the end point; can also use to meet the requirements of this standard other instruments.
The choice of instrument type and test conditions has a significant effect on the moisture detection results and should ensure that the instrument and operating conditions
The moisture content of the sample measured according to the method and the absolute difference between the moisture content of the sample measured according to the method of GB/T 6283
0.010%.
4.2 Aluminum sample tray.
5 sampling
According to GB/T 6678, GB/T 6679 in the relevant provisions.
6 Analysis steps
6.1 Preparation of the instrument
Open the instrument switch, preheat 30min; press the instrument manual input operating parameters. The following test conditions are recommended.
Heating temperature 110 ℃, standby temperature 105 ℃, slope 0.050%/2min, delay time 1s, sample volume of about 7 grams
When the plate diameter of 9.3cm).
6.2 Sample analysis
Place the empty sample tray (4.2) in the sample chamber of the heating module and return to the instrument after the instrument's quality reading is stable. Return the sample tray,
Add the right amount of sample, evenly spread in the sample tray, the sample should be taken to ensure that the sample is evenly laid and no exposed at the end of the disk.
Return the sample tray and weigh the sample. Press the instrument manual to operate the instrument, immediately test; instrument automatically detect the slope, when up to
When the preset value is reached, the instrument determines the end point. At this point the instrument automatically shows the moisture content of the sample.
Note. Depending on the instrument structure and heating performance, different sample sizes ......
Related standard:   SH/T 1499.4-2016  SH/T 1499.1-2012
   
 
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