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YC/T 146-2010Leaf tobacco - Threshing and redrying - Technical specification (English PDF)

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Issued by

State Tobacco Monopoly Bureau

Level / Type

National · Recommended

Issue date

January 25, 2010

Implementation date

February 1, 2010

Scope

YC/T 146-2010 (Leaf tobacco - Threshing and redrying - Technical specification) is available as an English-translated PDF.

YC/T 146-2010 — 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.

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Document preview — YC/T 146-2010

National Standard of the People's Republic of China

ICS
65.160
Classification
X 85

Issued by: State Tobacco Monopoly Bureau

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 µL.
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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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 10 pages — is available in the English PDF.

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