SJ/T 11634-2016 PDF English
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Determination of methanol in electronic industry with the developer -- Headspace gas chromatography method
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SJ/T 11634-2016: PDF in English (SJT 11634-2016) SJ/T 11634-2016
ELECTRONICS INDUSTRY STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
ICS 31.030
L 90
Record No.:
Determination of Methanol in Electronic Industry with
Developer – Headspace Gas Chromatography Method
ISSUED ON: APRIL 05, 2016
IMPLEMENTED ON: SEPTEMBER 01, 2016
Issued by: Ministry of Industry and Information Technology of PRC
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Terms and Definitions ... 4
4 Principle of Method ... 4
5 Reagents and Materials ... 5
6 Apparatus ... 6
7 Test ... 6
8 Precision and Results ... 7
9 Detection Limit of the Method ... 8
10 Spike Recovery Rate ... 9
11 Report ... 9
Determination of Methanol in Electronic Industry with
Developer - Headspace Gas Chromatography Method
1 Scope
This Standard specifies the method for the determination of methanol content in
developer for the electronics industry by headspace gas chromatography method.
This Standard is applicable to the determination of methanol content in developer for
the electronics industry. The minimum detection concentration of methanol in this
method is 1 mg/kg.
2 Normative References
The following documents are essential to the application of this document. For the
dated documents, only the versions with the dates indicated are applicable to this
document; for the undated documents, only the latest version (including all the
amendments) are applicable to this document.
GB/T 602 Chemical Reagent - Preparations of Standard Solutions for Impurity
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
GB/T 9722 Chemical Reagent - General Rules for the Gas Chromatography
3 Terms and Definitions
For the purpose of this document, the terms and definitions given in GB/T 9722 apply.
4 Principle of Method
In a closed bottle, at a certain temperature, methanol molecules escape from the liquid
phase to the gas phase. After a certain period of time, the methanol molecules reach
a dynamic equilibrium between the gas and liquid phases. At this time, the
concentration of methanol in the gas phase is proportional to its concentration in the
liquid phase. The methanol in the gas phase is separated by a capillary column and
detected by a hydrogen flame ionization detector. The retention time is qualitative, and
6 Apparatus
6.1 Gas chromatograph
Hydrogen flame ionization detector (FID) and data processing system.
6.2 Headspace sample-injecting device
Headspace sampler or other equivalent devices.
6.3 Headspace bottle
Commonly used volume is (22±0.5) mL; lined with polytetrafluoroethylene (PTFE) -
silicone rubber or butyl rubber pad and aluminum cap. Impurities that would disturb the
measurement of methanol shall not be generated in the pad.
6.4 Rolling and de-capping tools
Used to seal and open headspace bottles.
6.5 Perfluoroalkoxy resin (PFA) bottle
6.6 Electronic Balance
The minimum division value is 0.0001g.
7 Test
7.1 Reference conditions for instrument operation
7.1.1 Reference conditions for gas chromatograph operation
a) Chromatographic column type: polar capillary chromatographic column suitable
for separating methanol in the developer;
b) Carrier gas type: high-purity of nitrogen or helium;
c) Carrier gas flowrate: 1.5mL/min;
d) Detector type: hydrogen flame ionization detector;
e) Column temperature: 85°C;
f) Sampler temperature: 150°C;
g) Detector temperature: 300°C.
9 Detection Limit of the Method
Prepare the developer solution and developer solution quantitatively added 20mg/kg
methanol standard solution; adjust the instrument to the best working state; measure
the methanol content in the developer solution with/without adding methanol standard
solution; meanwhile, continuously measure at least for ten times.
The detection limit is calculated by "DL", the value is expressed by "mg/kg", and
calculated according to Formula (1):
Where:
C - The value of the concentration of methanol standard solution added to the
developer, in (mg/kg) [c = 20];
S - The standard deviation of the peak height or peak area of methanol in the developer
solution without adding the methanol standard solution;
S1 - The average peak height or peak area of methanol in the developer solution with
adding the methanol standard solution;
S0 - The average peak height or average area of methanol in the developer solution
without adding the methanol standard solution;
The standard deviation of the peak height or peak area of methanol in developer
solution without adding the methanol standard solution, expressed in terms of “s”, and
calculated by Formula (2):
Where:
xi – peak height or peak area of methanol in the developer with adding the methanol
standard solution;
– average peak height or peak area of methanol in the developer without adding the
methanol standard solution;
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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