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YC/T 332-2010 English PDF (YCT332-2010)

YC/T 332-2010 English PDF (YCT332-2010)

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YC/T 332-2010: Determination of formaldehyde in water-borne adhesives for cigarette - High performance liquid chromatographic method

This Standard specifies the determination of formaldehyde in water-borne adhesives for cigarette - High performance liquid chromatographic method.
YC/T 332-2010
YC
TOBACCO INDUSTRY STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 65.160
X 85
Record No. 27779-2010
Determination of formaldehyde in water-borne
adhesives for cigarette -
High performance liquid chromatographic method
ISSUED ON. JANUARY 25, 2010
IMPLEMENTED ON. FEBRUARY 1, 2010
Issued by. State Tobacco Monopoly Bureau
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principle... 4
4 Reagents ... 4
5 Material and apparatus ... 6
6 Analysis steps ... 6
7 Results calculation and representation ... 8
8 Recovery rate, detection limit and quantitation limit ... 8
9 Test report ... 9
Appendix A ... 10
Foreword
This Part was drafted in accordance with the rules given in GB/T 1.1-2009. This Standard was proposed by State Tobacco Monopoly Bureau.
This Standard shall be under the jurisdiction of National Technical Committee on Tobacco of Standardization Administration of China (SAC/TC 144/SC 8). The drafting organizations of this Standard. China Research Centre for Tobacco, China Tobacco Hunan Industrial Co., Ltd., Shanghai Tobacco (Group) Company, Hongyun Honghe Tobacco (Group) Co., Ltd., and National Tobacco Quality
Supervision and Inspection Center.
Main drafters of this Standard. Dai Yunhui, Jiang Lamei, Wu Mingjian, Chen Lianfang, Han Yunhui, Wu Da, Tang Gangling, Zhan Jianbo, Xia Jianjun, Liao Tougen and Chen Chen.
Determination of formaldehyde in water-borne
adhesives for cigarette -
High performance liquid chromatographic method
1 Scope
This Standard specifies the determination of formaldehyde in water-borne adhesives for cigarette - High performance liquid chromatographic method. This Standard is applicable to the determination of formaldehyde in water-borne adhesives for cigarette.
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 6682 Water for analytical laboratory use - Specification and test
methods (GB/T 6682-2008, ISO 3696.1987, MOD)
3 Principle
Use water to dilute the formaldehyde in the extracted sample. After
formaldehyde hydrazine is derived from 2,4-dinitrophenylhydrazine, use HPLC (high performance liquid chromatograph) / diode array detector to determine, and quantify by external-standard method.
4 Reagents
In addition to special requirements, all reagents are analytical pure. The water shall comply with the requirements for Grade-1 in GB/T 6682.
4.1 Reagents
4.1.1 Acetonitrile (chromatographic pure).
If the concentration of sample solution for test exceeds the concentration range of standard working curve, make appropriate adjustment to pretreatment of sample before re-determining it.
6.2 Blank test
Do not add sample. Repeat 6.1 and conduct HPLC analysis.
6.3 Apparatus conditions
6.3.1 Column temperature. 30??C.
6.3.2 Flow speed. 0.5 mL/min.
6.3.3 Injection volume. 10 ??L.
6.3.4 Detection wavelength. 352.0 nm.
6.3.5 Mobile phrase. A is water and B is acetonitrile (4.1.1).
6.3.6 Gradient elution procedure. shown in Table 2.
Table 2 Gradient elution procedure
Time
min
Mobile phrase A
Mobile phrase B
0.00 70 30
5.00 10 90
15.00 10 90
16.00 70 30
20.00 70 30
6.4 Drawing of standard working curve
Respectively take standard solutions (4.2) to conduct HPLC analysis. The standard working curve of formaldehyde shall be based on the standard
solution concentration and formaldehyde response peak area. The linear
correlation coefficient of working curve is R2 >0.99.
Standard curve shall be made for each test. After determination of every 20 samples, it shall add a standard solution of medium solution. If the difference between the determined value and the original value exceeds 3%, it shall re- draw the standard curve.
6.5 Sample determination
Determine the sample (6.1) based on apparatus?€? conditions. Determine the nature according to retention time. Use external-standard method to quantify. Repeat the determination twice for each sample. Conduct a group of blank test for each batch of sample. Refer to Appendix A for chromatogram of standard solution and sample derived solution.
7 Results calculation and representation
The content of formaldehyde in the sample shall be calculated according to equation (1).
Where,
X - Content of formaldehyde in the sample, in milligrams per kilogram
(mg/kg);
c - Formaldehyde concentration obtained by standard curve, in milligrams per liter (mg/L);
c0 - Blank value obtained by standard curve, in milligrams per liter (mg/L); V - Volume of extracted solution, in milliliters (mL);
m - Sample material mass, in grams (g);
S - Dilution factor of sample solution.
Take the average of two parallel determinations as the final result, accurate to 0.1 mg/kg.
Relative mean deviation of two parallel determinations shall be less than 10%. 8 Recovery rate, detection limit and quantitation limit
The recovery rate, detection limit and quantitation limit of this method are shown in Table 3.
Table 3 Recovery rate, detection limit and quantitation limit of this
method
Compound Recovery rate %
Detection limit
mg/kg
Quantitation limit
mg/kg
Formaldehyde 91.0~105.7 1.6 5.3
9 Test report
The test report shall contain at least the following information.
- All information necessary for identification of sample for test;
- Test methods used that are referenced by this Standard;
- Determination results, including results and average value of each single determination;
- Differences with analysis steps stipulated by this Standard;
- Any anomalies observed during the test;
- The date of the test;
- Test personnel.

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