GB/T 15336-2013 English PDF (GBT15336-2013)

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GB/T 15336-2013: Phthalic anhydride
GB/T 15336-2013
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.01; 87.060.10
G 56
Replacing GB/T 15336-2006
Phthalic anhydride
邻苯二甲酸酐
ISSUED ON. JULY 19, 2013
IMPLEMENTED ON. DECEMBER 01, 2013
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
1 Scope ... 4 
2 Normative references ... 4 
3 Requirements ... 5 
4 Safety information ... 6 
5 Sampling ... 6 
6 Test methods ... 6 
7 Inspection rules ... 12 
8 Marking, labelling, transportation and storage ... 13 
Foreword
This Standard is drafted in accordance with the rules provided in GB/T 1.1-2009.
This Standard replaces GB/T 15336-2006 “Phthalic anhydride”; compared with GB/T
15336-2006, the main technical changes, other than editorial changes, are as follows.
— Add CAS No. (see chapter 1);
— Add technical indicators and inspection methods for determination of purity through
gas chromatographic method (see chapter 3; 5.9);
— Delete technical indicators and inspection methods for determination of phthalic
anhydride content through chemical method in original standard (chapter 3 and 5.7
of edition 2006).
— Revise the indicators of superior products on sulfuric acid colour No. (see chapter 3;
3 of edition 2006);
— Delete the technical indicators and test methods of ash content in original standard
(chapter 3 and chapter 6 of edition 2006);
— Revise crystallization point to type inspection items (see 7.1; 7.1 of edition 2006);
— Add “safety information” (see chapter 4).
This Standard was proposed by Chine Petroleum and Chemical Industry Federation.
This Standard shall be under the jurisdiction of National Technical Committee on Dyestuff
of Standardization Administration of China (SAC/TC 134).
Drafting organizations of this Standard. The Organic Chemical Co., Ltd. of Tongling
Chemical Industry Group Corporation AND Shenyang Research Institute of Chemical
Industry Co., Ltd.
Main drafters of this Standard. Yang Jiaren, Yang Jiemin and Cao Wenlian.
Previous versions replaced by this Standard are as follows.
- GB/T 15336-1994, GB/T 15336-2006.
Phthalic anhydride
Warning — Personnel that use this Standard shall have practical
experience in normalized laboratory. This Standard does not indicate all
possible safety issues. Users have the responsibilities to take appropriate
safety and health measures, and ensure the conformity to relevant
national laws and regulations.
1 Scope
This Standard specifies the phthalic anhydride’s requirements, safety information,
sampling, test methods, inspection rules, marking, labelling, packaging, transportation and
storage.
This Standard applies to product quality control of phthalic anhydride.
Structural formula.
Molecular formula. C8H4O3
Relative molecular mass. 148.12 (based on international relative atomic mass in 2009)
CAS RN. 85-44-9
2 Normative references
The following documents are indispensable for application of this document. For the dated
documents so quoted, only the dated versions apply to this document. For the undated
documents so quoted, the latest versions (including all modification sheets) apply to this
document.
GB190 Packing symbol of dangerous goods
GB/T 191 Packaging - Pictorial markings for handling of goods (GB/T 191-2008, ISO
780.1997, MOD)
GB/T 601 Chemical reagent - Preparations of standard volumetric solutions
4 Safety information
4.1 Safety
According to GB/T2268-2012, phthalic anhydride belongs to the eighth category of
corrosive substances; hazardous material No. is UN. 2214 (CN. 81631). It stimulates eyes
and skins, and contact with the skin may cause allergies. Necessary protective measures
shall be taken during use and handling, so as to avoid contact with eyes and skins; pay
close attention to safety.
4.2 Safety technical instructions
According to GB/T 16483, this product shall be accompanied with detailed safety technical
instructions during delivery, which shall include following contents.
a) Providing risk information of this product;
b) Safe application method;
c) Transportation and storage requirements;
đ) Protective measures;
e) Emergency measures, etc.
5 Sampling
Sampling is based on batches; uniform-products for each inspection are regarded as one
batch. The number of samples for each batch shall conform to the provisions in 7.6 of GB/T
6678-2003. Packages of all samples shall be intact; be sure to prevent foreign matters
from falling into products. During sampling, use a probe tube to take samples from three
parts of the upper, middle and lower; total amount of samples taken shall not be less than
500 g; respectively put into two clean, dry and well-sealed containers after sufficiently
mixing the samples taken; affix with labels. Indicate the product name, batch No., name of
manufacturer, sampling date and place. One sample for inspection; the other one for future
reference.
6 Test methods
6.1 General provisions
Unless otherwise specified, only use reagents that are verified analytically pure and Grade-
3 water prescribed in GB/T 6682-2008. When there is no other requirement, the standard
titration solutions, preparations and products used in test shall be prepared and calibrated
according to the provisions of GB/T 601 and GB/T 603; determination of inspection results
are based on rounding-value comparison method in 4.4.3 of GB/T 8170-2008.
same volume (colorimetric method is same as 6.3).
6.4.2 Tolerance
The same as 6.3.3.
6.5 Determination of sulfuric acid chromaticity
6.5.7 Determination steps
Weigh 2 g of fine phthalic anhydride sample (accurate to 0.1 g); place into a dry and clean
colorimetric tube; add sulfuric acid to 25 mL; shake until the sample is completely dissolved;
make it stand for 20 min; compare with chromaticity standard solution of the same volume
along axial direction (colorimetric method is same as 6.3).
6.5.2 Tolerance
The same as 6.3.3.
6.6 Determination of crystallizing point
Conduct in accordance with the provisions of GB/T 2385.
6.7 Determination of phthalic anhydride purity
6.7.1 Determination principles
Adopt gas chromatographic method; the sample is separated through capillary
chromatographic column; detected by flame ionization detector; and measured through
peak area normalization method.
6.7.2 Reagents
Acetone. Chromatographically pure.
6.7.3 Instruments and equipment
a) Gas chromatograph. Instrument sensitivity and stability shall conform to the
provisions of 6.3 and 6.4 in GB/T 9722-2006.
b) Detector. Flame ionization detector (FID);
c) Chromatographic work station or integrator;
d) Micro-injector. 1.0μL~10.0μL;
e) Chromatographic column. Length is 30 m, inner diameter is 0.32 mm, film thickness
is 0.25μm, stationary phase is (50% phenyl)-methylpolysilicone (e.g. DB-17 or other
capillary columns that can achieve the same separation effect).
7.2 Exit-factory inspection
Phthalic anhydride shall pass the inspection by quality inspection department of the
manufacturer and may be delivered only after certificate of quality has been attached.
Manufacturer shall ensure that all delivered products conform to requirements of this
Standard.
7.3 Re-inspection
If one indicator in inspection results does not conform to this Standard, it is necessary to
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