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QB/T 5291-2018 PDF English

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QB/T 5291-2018: Determination of hexavalent chromium in cosmetics
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QB/T 5291-2018: Determination of hexavalent chromium in cosmetics

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LIGHT INDUSTRY STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.100.70 Classification No.. Y42 Filing No.. 65903-2018 Determination of hexavalent chromium in cosmetics Issued on. OCTOBER 22, 2018 Implemented on. APRIL 01, 2019 Issued by. Ministry of Industry and Information Technology of PRC

Table of Contents

Foreword... 3 Introduction... 4 1 Scope... 5 2 Normative references... 5 3 Method 1 -- Diphenylcarbazide spectrophotometry... 5 4 Method 2 -- Ion chromatography-inductively coupled plasma mass spectrometry... 8 Appendix A (Informative) Reference conditions of instrument... 12 Appendix B (Informative) Ion chromatography-mass spectrograms of standard solutions and samples... 13

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard was proposed by China National Light Industry Federation. This standard shall be under the jurisdiction of the National Standardization Technical Committee of Flavor, Flavor and Cosmetics (SAC/TC 257). Drafting organizations of this standard. Dalian Institute of Product Quality Inspection (National Center for Quality Supervision and Inspection of Daily Chemical Products), Dalian Food Inspection Institute, Shanghai Institute of Daily Chemical Industry (National Center for Quality Supervision and Inspection of Flavor and Cosmetics). The main drafters of this standard. Zhao Tong, Mao Xiqin, Shen Min, Zhou Huimin, Niu Jinhui, Cai Qiang, Jia Zhenqiang. This standard is published for the first time.

1 Scope

This standard specifies the methods for the determination of hexavalent chromium in cosmetics, by diphenylcarbazide spectrophotometry and ion chromatography- inductively coupled plasma mass spectrometry. This standard applies to the determination of hexavalent chromium in cosmetics. When the sample weight is 2 g, the detection limit of diphenylcarbazide spectrophotometry is 0.25 mg/kg, the quantification limit is 0.83 mg/kg; the detection limit of ion chromatography-inductively coupled plasma mass spectrometry is 0.010 mg/kg, the quantification limit is 0.033 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) is applicable to this standard. GB/T 6682 Water for analytical laboratory use - Specification and test methods

3 Method 1 -- Diphenylcarbazide spectrophotometry

3.1 Principle After the sample is extracted by the alkaline leaching solution, the hexavalent chromium in the leaching solution reacted with diphenylcarbazide in an acidic solution, to form a purple-red complex, which was determined by spectrophotometry, at a wavelength of 540 nm. 3.2 Reagents Unless otherwise specified, the reagents are of analytical grade. The water is the first grade water, which is specified in GB/T 6682. 3.3 Instruments 3.4 Analytical procedures 3.5 Result calculation Calculate the hexavalent chromium, X, in the specimen, according to formula (1). 3.6 Recovery and precision When the standard addition concentration is in the range of 0.5 mg/L ~ 10.0 mg/L, the recoveries are in the range of 88.4% ~ 102.9%, the precisions are in the range of 1.9% ~ 7.1%. 3.7 Tolerance The absolute difference, between the results of two independent determinations, which are obtained under repeatability conditions, shall not exceed 10% of the arithmetic mean.

4 Method 2 -- Ion chromatography-inductively coupled plasma mass spectrometry

4.1 Principle After the samples are extracted with alkaline leaching solution, the leaching solution is determined by ion chromatography-inductively coupled plasma mass spectrometry, AND quantified by external standard method. 4.2 Reagents Unless otherwise specified, the reagents are of analytical grade. The water is the first grade water, which is specified in GB/T 6682. 4.3 Instruments and equipment 4.3.1 Ion chromatography-inductively coupled plasma mass spectrometer. 4.3.2 Ultrasonic generator. Constant temperature (60 ± 1) °C. 4.3.3 Analytical balance. Sensitivity 0.0001 g. 4.3.4 Graduated centrifuge tube (polyethylene or polypropylene). Specification 50 mL. 4.4 Analytical procedures 4.4.1 Pre-treatment of sample Accurately weigh (0.5 g ~ 2 g, accurate to 0.0001 g) of the sample, into a 50 mL graduated centrifuge tube. Add 20.0 mL of extract (4.2.8) and 0.5 mL of buffer (4.2.9). Completely submerge the sample in the extract. Shake well. Carry out ultrasonic extraction, at 60 °C for 20 min. Take it out. After cooling to room temperature, use water to make the volume to 25.0 mL. Add 2.0 g of activated carbon powder. Shake well. Use filter paper to filter it. Discard the first 1 mL of filtrate. Collect the filtrate. Use microporous filter membrane (4.2.13) to filter the collected filtrate. Prepare for determination. Meanwhile do a reagent blank test. 4.4.3 Determination The instrument is tuned and set, to measure the standard curve solution, reagent blank solution, sample solution in sequence. See Appendix A, for instrument reference conditions. 4.6 Recovery and precision When the standard concentration is in the range of 0.10 mg/kg ~ 10 mg/kg, the recovery rate is 86.0% ~ 103.7% AND the precision is in the range of 1.1% ~ 8.1%. 4.7 Tolerance The absolute difference, between the results of two independent determinations, which are obtained under repeatability conditions, is not more than 10 % of the arithmetic mean.

Appendix A

(Informative) Reference conditions of instrument A.1 Ion chromatography conditions The ion chromatography conditions are as follows. A.2 Inductively coupled plasma mass spectrometry conditions Inductively coupled plasma mass spectrometry conditions are as follows.

Appendix B

(Informative) Ion chromatography-mass spectrograms of standard solutions and samples See Figure B.1 and Figure B.2, for the ion chromatogram-mass spectrum of the standard solution and sample. QB/T 5291-2018 LIGHT INDUSTRY STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 71.100.70 Classification No.. Y42 Filing No.. 65903-2018 Determination of hexavalent chromium in cosmetics Issued on. OCTOBER 22, 2018 Implemented on. APRIL 01, 2019 Issued by. Ministry of Industry and Information Technology of PRC

Table of Contents

Foreword... 3 Introduction... 4 1 Scope... 5 2 Normative references... 5 3 Method 1 -- Diphenylcarbazide spectrophotometry... 5 4 Method 2 -- Ion chromatography-inductively coupled plasma mass spectrometry... 8 Appendix A (Informative) Reference conditions of instrument... 12 Appendix B (Informative) Ion chromatography-mass spectrograms of standard solutions and samples... 13

Foreword

This standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard was proposed by China National Light Industry Federation. This standard shall be under the jurisdiction of the National Standardization Technical Committee of Flavor, Flavor and Cosmetics (SAC/TC 257). Drafting organizations of this standard. Dalian Institute of Product Quality Inspection (National Center for Quality Supervision and Inspection of Daily Chemical Products), Dalian Food Inspection Institute, Shanghai Institute of Daily Chemical Industry (National Center for Quality Supervision and Inspection of Flavor and Cosmetics). The main drafters of this standard. Zhao Tong, Mao Xiqin, Shen Min, Zhou Huimin, Niu Jinhui, Cai Qiang, Jia Zhenqiang. This standard is published for the first time.

1 Scope

This standard specifies the methods for the determination of hexavalent chromium in cosmetics, by diphenylcarbazide spectrophotometry and ion chromatography- inductively coupled plasma mass spectrometry. This standard applies to the determination of hexavalent chromium in cosmetics. When the sample weight is 2 g, the detection limit of diphenylcarbazide spectrophotometry is 0.25 mg/kg, the quantification limit is 0.83 mg/kg; the detection limit of ion chromatography-inductively coupled plasma mass spectrometry is 0.010 mg/kg, the quantification limit is 0.033 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) is applicable to this standard. GB/T 6682 Water for analytical laboratory use - Specification and test methods

3 Method 1 -- Diphenylcarbazide spectrophotometry

3.1 Principle After the sample is extracted by the alkaline leaching solution, the hexavalent chromium in the leaching solution reacted with diphenylcarbazide in an acidic solution, to form a purple-red complex, which was determined by spectrophotometry, at a wavelength of 540 nm. 3.2 Reagents Unless otherwise specified, the reagents are of analytical grade. The water is the first grade water, which is specified in GB/T 6682. 3.3 Instruments 3.4 Analytical procedures 3.5 Result calculation Calculate the hexavalent chromium, X, in the specimen, according to formula (1). 3.6 Recovery and precision When the standard addition concentration is in the range of 0.5 mg/L ~ 10.0 mg/L, the recoveries are in the range of 88.4% ~ 102.9%, the precisions are in the range of 1.9% ~ 7.1%. 3.7 Tolerance The absolute difference, between the results of two independent determinations, which are obtained under repeatability conditions, shall not exceed 10% of the arithmetic mean.

4 Method 2 -- Ion chromatography-inductively coupled plasma mass spectrometry

4.1 Principle After the samples are extracted with alkaline leaching solution, the leaching solution is determined by ion chromatography-inductively coupled plasma mass spectrometry, AND quantified by external standard method. 4.2 Reagents Unless otherwise specified, the reagents are of analytical grade. The water is the first grade water, which is specified in GB/T 6682. 4.3 Instruments and equipment 4.3.1 Ion chromatography-inductively coupled plasma mass spectrometer. 4.3.2 Ultrasonic generator. Constant temperature (60 ± 1) °C. 4.3.3 Analytical balance. Sensitivity 0.0001 g. 4.3.4 Graduated centrifuge tube (polyethylene or polypropylene). Specification 50 mL. 4.4 Analytical procedures 4.4.1 Pre-treatment of sample Accurately weigh (0.5 g ~ 2 g, accurate to 0.0001 g) of the sample, into a 50 mL graduated centrifuge tube. Add 20.0 mL of extract (4.2.8) and 0.5 mL of buffer (4.2.9). Completely submerge the sample in the extract. Shake well. Carry out ultrasonic extraction, at 60 °C for 20 min. Take it out. After cooling to room temperature, use water to make the volume to 25.0 mL. Add 2.0 g of activated carbon powder. Shake well. Use filter paper to filter it. Discard the first 1 mL of filtrate. Collect the filtrate. Use microporous filter membrane (4.2.13) to filter the collected filtrate. Prepare for determination. Meanwhile do a reagent blank test. 4.4.3 Determination The instrument is tuned and set, to measure the standard curve solution, reagent blank solution, sample solution in sequence. See Appendix A, for instrument reference conditions. 4.6 Recovery and precision When the standard concentration is in the range of 0.10 mg/kg ~ 10 mg/kg, the recovery rate is 86.0% ~ 103.7% AND the precision is in the range of 1.1% ~ 8.1%. 4.7 Tolerance The absolute difference, between the results of two independent determinations, which are obtained under repeatability conditions, is not more than 10 % of the arithmetic mean.

Appendix A

(Informative) Reference conditions of instrument A.1 Ion chromatography conditions The ion chromatography conditions are as follows. A.2 Inductively coupled plasma mass spectrometry conditions Inductively coupled plasma mass spectrometry conditions are as follows.

Appendix B

(Informative) Ion chromatography-mass spectrograms of standard solutions and samples See Figure B.1 and Figure B.2, for the ion chromatogram-mass spectrum of the standard solution and sample. ......

Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
Image 1     Image 2     Image 3     

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