GB/T 1677-2023 English PDF (GBT1677-2023)

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GB/T 1677-2023: Determinating the epoxy value of plasticizers
GB/T 1677-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 71.100.40
CCS G 70
Replacing GB/T 1677-2008
Determining the epoxy value of plasticizers
ISSUED ON. DECEMBER 28, 2023
IMPLEMENTED ON. JULY 01, 2024
Issued by. State Administration for Market Regulation;
Standardization Administration of the People's Republic of China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative references... 5
3 Terms and definitions... 5
4 Reagents and solutions... 5
5 Instruments... 6
6 Test methods... 6
Annex A (informative) Preparation method of sodium hydroxide standard titration
solution (0.15 mol/L)... 9
Foreword
This document was drafted in accordance with the rules given in GB/T 1.1-2020
"Directives for standardization - Part 1.Rules for the structure and drafting of
standardizing documents".
This document replaces GB/T 1677-2008 "Determination the epoxy value of
plasticizers". Compared with GB/T 1677-2008, in addition to structural adjustments
and editorial changes, the main technical changes in this document are as follows.
a) Change the scope of the content (see Chapter 1 of this Edition; Chapter 1 of
Edition 2008);
b) Add potassium hydrogen phthalate [CAS No.. 877-24-7] reference reagent and its
requirements (see 4.4 of this Edition);
c) Delete the contents of pyridine and hydrochloric acid-pyridine solution (see 4.3
and 4.5 of Edition 2008);
d) Change the content of sodium hydroxide standard titration solution (see 4.6 of
this Edition; 4.7 of Edition 2008);
e) Add instrument pipette (see 5.3 of this Edition). Delete instrument volumetric
flask, straight condenser and oil bath (see 5.2, 5.4 and 5.5 of Edition 2008);
f) Delete Method B for determination of epoxy value (see Chapter 6 of Edition 2008);
g) Add the epoxy value determination method of hydrochloric acid-acetone-
phenolphthalein method (see 6.1.2 of this Edition);
h) Add the acid value determination method (see 6.2 of this Edition).
Attention is drawn to the possibility that some of the elements of this document may be
the subject of patent rights. The issuing authority shall not be held responsible for
identifying any or all such patent rights.
This document was proposed by China Petroleum and Chemical Industry Federation.
This document shall be under the jurisdiction of National Technical Committee on
Rubber and Rubber Products of Standardization Administration of China (SAC/TC 35).
The drafting organizations of this document. Shanxi Chemical Research Institute (Co.,
Ltd.), Zhejiang Jiaao Environmental Protection Technology Co., Ltd., Xinjinlong Bio-
based Materials (Hubei) Co., Ltd., Shandong Kexing Chemical Co., Ltd., Nantong
Haierma Technology Co., Ltd., and Xiamen University.
Determining the epoxy value of plasticizers
IMPORTANT NOT. People who use this document shall have practical experience
in formal laboratory work. This document does not point out all possible safety
issues. Users are responsible for taking appropriate safety and health measures
and ensuring that the conditions stipulated by relevant national laws and
regulations are met.
1 Scope
This document describes the test method for the epoxy value of a range of epoxy
plasticizers.
This document is applicable to the determination of epoxy value of epoxy plasticizer
series products.
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 601, Chemical reagent -- Preparations of reference titration solutions
GB/T 603, Chemical reagent -- Preparations of reagent solutions for use in test
methods
GB 1257, Working chemicals -- Potassium hydrogen phthalate
GB/T 6682, Water for analytical laboratory use -- Specification and test methods
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1 epoxy value
The oxygen content of epoxy groups per 100 g of specimen.
4 Reagents and solutions
Unless otherwise specified, only analytically-pure reagents and grade 3 water that
complies with GB/T 6682 are used in the analysis.
The standard titration solutions and products used in the analysis shall be prepared in
accordance with GB/T 601 and GB/T 603 unless other requirements are specified.
4.1 Hydrochloric acid [CAS No.. 7647-01-0].
4.2 Acetone [CAS No.. 67-64-1].
4.3 Ethanol [CAS No.. 64-17-5]. 95%.
4.4 Potassium hydrogen phthalate [CAS No.. 877-24-7] standard reagent. in accordance
with the requirements of GB 1257.
4.5 Hydrochloric acid-acetone solution. the volume ratio of hydrochloric acid and
acetone is 1.40.Store in a sealed glass bottle and prepare before use.
4.6 Standard sodium hydroxide titration solution. c NaOH = 0.01 mol/L, c NaOH = 0.1
mol/L, c NaOH = 0.15 mol/L (see Annex A for the preparation method).
4.7 Phenolphthalein [CAS No.. 77-09-8] Indicator solution. 10 g/L. Weigh 1 g of
phenolphthalein and dissolve it in 95% ethanol. Make up to 100 mL with 95% ethanol.
4.8 Cresol red indicator solution. 1 g/L. Weigh 0.1 g of cresol red, accurate to 0.0001 g.
Add 26 mL of 0.1 mol/L sodium hydroxide. Dissolve and dilute to 100 mL with distilled
water.
4.9 Thymol blue indicator solution. 1 g/L. Weigh 0.1 g of thymol blue, accurate to
0.0001 g. Add 22 mL of 0.01 mol/L sodium hydroxide. After dissolving, add distilled
water to dilute to 100 mL.
4.10 Mixed indicator solution. Take 10 mL of cresol red indicator solution. Add 30 mL
of thymol blue indicator solution. Mix well. Adjust to neutral with 0.01 mol/L sodium
hydroxide and 0.01 mol/L hydrochloric acid solution (the mixed indicator changes color
at about pH=9.8).
5 Instruments
5.1 Conical flask with stopper. 250 mL.
5.2 Alkaline burette. 50 mL, with the graduation of 0.1mL.
5.3 Pipette. 20 mL.
6 Test methods
6.1 Sample determination
Annex A
(informative)
Preparation method of sodium hydroxide standard titration solution (0.15
mol/L)
A.1 Preparation
Weigh 6 g of sodium hydroxide and dilute to 1000 mL with water. Shake well and set
aside for later use.
A.2 Calibration
Weigh 3 portions of approximately 1 g each (accurate to 0.0001 g) and dry to a constant
amount of potassium hydrogen phthalate standard reagent at 105℃±2℃. Dissolve it in
carbon dioxide-free water and make up to 50 mL. Use phenolphthalein as an indicator.
Titrate with the sodium hydroxide standard titration solution to be calibrated until it
turns pink. Keep for 30 s. The volume consumed is V1.Perform a blank test at the same
time. Take 50 mL of carbon dioxide-free water. Titrate with the sodium hydroxide
standard titration solution to be calibrated until it turns pink. Keep for 30 s. The volume
consumed is V0.
A.3 Result calculation
The concentration of sodium hydroxide standard titration solution is calculated as
shown in formula (A.1).
Where,
c NaOH - the concentration of sodium hydroxide standard titration solution, in moles per
liter (mol/L);
m1 – the mass of potassium hydrogen phthalate, in grams (g);
V1 - the volume of sodium hydroxide standard titration solution consumed for
calibration, in milliliters (mL);
V0 - the volume of sodium hydroxide standard titration solution consumed for
calibration, in milliliters (mL);
204.22 - the molar mass of potassium hydrogen ph...