GBZT313.2-2018 English PDF

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GBZT313.2-2018: Determination of trimethyltin chloride (TMT) in urine -- Part 2: Gas chromatographic mass method
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GBZ/T 313.2-2018	139	Add to Cart	3 days	Determination of trimethyltin chloride (TMT) in urine -- Part 2: Gas chromatographic mass method	Valid

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GBZ 20   GBZ 57   GBZ 49   GBZ/T 329   GBZ/T 330   GBZ/T 313.1   

Basic data

Standard ID: GBZ/T 313.2-2018 (GBZ/T313.2-2018)
Description (Translated English): Determination of trimethyltin chloride (TMT) in urine -- Part 2: Gas chromatographic mass method
Sector / Industry: National Standard (Recommended)
Classification of Chinese Standard: C60
Word Count Estimation: 7,729
Date of Issue: 2018-08-16
Date of Implementation: 2019-01-01
Regulation (derived from): State-Health-Communication (2018) No.14
Issuing agency(ies): National Health and Family Planning Commission

GBZ/T 313.2-2018: Determination of trimethyltin chloride (TMT) in urine -- Part 2: Gas chromatographic mass method

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Determination of trimethyltin chloride (TMT) in urine - Part 2. Gas chromatographic–mass method ICS 13.100 C 52 National Occupational Health Standards Determination of trimethyltin chloride in urine Part 2. Gas chromatography-mass spectrometry Determination of trimethyltin chloride (TMT) in urine-- Part 2. Gas chromatographic–mass method 2018 - 08 - 16 released 2019 - 01 - 01 Implementation National Health and Wellness Committee of the People's Republic of China

Foreword

This standard is formulated in accordance with the Law of the People's Republic GBZ /T 312 "Determination of Trimethyltin Chloride in Urine" is divided into two parts. -- Part 1. Gas chromatography; -- Part 2. Gas chromatography-mass spectrometry. This part is the second part of GBZ /T 313. This part is drafted in accordance with the rules given in GB/T 1.1-2009. This section drafted by. Guangdong Provincial Occupational Disease Prevention and Control Institute, Shenzhen Occupational Disease Prevention and Control Institute, Shenzhen Luohu District Center for Disease Control and Prevention, Shenzhen Longgang District Center for Disease Control and Prevention. The main drafters of this section. Wu Banghua, Yan Weifeng, Yi Juan, Lai Shaoyang, Liu Li, He Jiaheng, Wu Chuan, Cai Jinmin, Xie Yuzhen, Liu Fen, He Juntao, Lai Yiqi, Zhang Ying, Cai Zhibin, Liu Qu, Zhang Wen, Lin Yiran, Yan Jianpei, Zhang Ying. Determination of trimethyltin chloride in urine - Part 2. Gas chromatography - mass spectro

1 Scope

This part of GBZ /T 313 specifies gas chromatography-mass spectrometry for the determination of trimethyltin chloride in urine. This section applies to the determination of trimethyltin chloride in the urine of occupational contacts.

2 Normative references

The following documents are indispensable for the application of this document. For dated references, only the dated version applies to this article. Pieces. For undated references, the latest edition (including all amendments) applies to this document. General rules for biological monitoring of GBZ /T 295 occupational population WS/T 97 urinary creatinine spectrophotometric method WS/T 98 urinary creatinine by reversed-phase high performance liquid chromatography

3 Principle

Trimethyltin chloride in the urine is derivatized with sodium tetraethylborate to trimethylethyltin, extracted with n-hexane, and detected by gas chromatography-mass spectrometry. It was characterized by the retention time and the abundance ratio of the characteristic ions, and quantified by the ion abundance value (peak area) of the characteristic ions of 165 m/z.

4 instruments

4.1 stoppered polyethylene plastic bottle, 50mL. 4.2 Centrifuge, 0 r/min ~ 3000r/min. 4.3 Microinjector, 1μL, 10μL, 50μL, 100μL. 4.4 Plug glass tube. 15mL with PTFE sealing cap. 4.5 vortex oscillator. 4.6 Gas Chromatography-Mass Spectrometer. Instrument operation reference conditions. a) Chromatographic conditions. - Column. 60 m × 0.32 mm × 1.0 μm Diphenyl-95% dimethyl siloxane copolymer (HP-5MS); - Column temperature. initial temperature 50 °C, rise to.200 °C at 20 °C/min, keep 1.0min; -- vaporization chamber temperature. 250 ° C; -- Column flow. 2.0 mL/min; - Split ratio. 5. 1. b) Mass spectrometry conditions. --Ion source. electron bombarded ion source (EI); --Ionization energy. 70eV; --Ion source temperature. 230 °C; -- Interface temperature. 260 ° C; -- Scan mode. Select ion scan mode, select 165 m/z as quantitative ion, 151m/z, 165m/z, 179m/z and 194 m/z To identify ions; -- Solvent delay time. 4.0 min.

5 reagent

5.1 The experimental water is deionized water. 5.2 Trimethyltin chloride, excellent grade ( >99.8%). 5.3 sodium tetraethyl borate, excellent grade pure. 5.4 Tetrahydrofuran, analytically pure. 5.5 Sodium acetate, analytically pure. 5.6 Glacial acetic acid, analytically pure. 5.7 n-hexane, chromatographically pure. 5.8 Derivatizing agent. Weigh 0.1 g of sodium tetraethyl borate and dissolve it in 10 mL of tetrahydrofuran to prepare 1% sodium tetraethylborate-tetrahydrofuran. The solution is stored in a refrigerator at 4 ° C in the dark and stable for 1 month. 5.9 Buffer (pH 4.0 ± 0.2). Add 0.6 g of sodium acetate to 120 mL of water, followed by 1.4 mL of glacial acetic acid. 5.10 Standard solution. Add a small amount of water to a 10mL volumetric flask. After weighing accurately, add a certain amount of trimethyltin chloride. Weighing, add water to the scale; calculate the concentration of this solution from the difference of 2 weighings, which is the standard stock solution (concentration is about 5mg/mL), this solution is at 4°C It can be stored in the refrigerator for 6 months. Dilute to 50.0 μg/mL Trimethyltin chloride standard solution with water before use. Or purchase certified by the state and A standard solution substance that is awarded a standard substance certificate. 6 Sample collection, transportation and storage A 50-mL random urine sample of workers exposed to trimethyltin chloride is collected in a polyethylene plastic bottle and transported at room temperature or refrigerated. Store in a 4°C refrigerator and store samples for 15 days.

7 Analysis steps

7.1 Determine urinary creatinine concentration by WS/T 97 or WS/T 98. 7.2 Sample treatment. Shake the urine sample, pipette 5.0 mL of urine sample into 15 mL stoppered glass tube, and add 5.0 mL buffer solution and 0.2 mL respectively. The derivatizing agent and 1.0 mL of n-hexane were shaken in a vortex shaker for 5 min. After standing or centrifuging, the upper organic phase was analyzed by 1.0 μL. If The concentration of trimethyltin chloride in the sample exceeds the measurement range, and it can be measured by diluting with n-hexane. The calculation is multiplied by the dilution factor. 7.3 Reagent blank treatment. replace the urine sample with 5.0mL water, and treat the sample as the reagent blank. 7.4 Preparation and determination of standard series of solutions. Add 5.0 mL of water to a 15 mL glass tube, and add standard solution to prepare A standard solution of trimethyltin chloride in the range of 0.0g to 2.5g, and 5.0 mL of buffer, 0.2 mL in each standard series solution. The derivatizing agent and 1.0 mL of n-hexane were shaken in a vortex shaker for 5 min, and after standing or centrifuging, the upper organic phase was analyzed by 1.0 μL. Reference According to the operating conditions of the instrument, the gas chromatograph-mass spectrometer was adjusted to the optimal measurement state, and 1.0 μL of the n-hexane extract was separately injected to measure each. Standard series of solutions. The measured ion abundance value (peak area) of the 165m/z characteristic ion is plotted against the corresponding trimethyltin chloride content (g) Make a standard curve or calculate a regression equation. 7.5 Sample determination. Determination of the ion abundance value of the sample and reagent blanks at 165 m/z using the operating conditions of the standard series of solutions (peak surface) Product), the content of trimethyltin chloride (g) is obtained from a standard curve or a regression equation.

8 calculation

Calculate the concentration of trimethyltin chloride in urine according to formula (1). kDV  (1) In the formula. C--the concentration of trimethyltin chloride in urine, in micrograms per gram of creatinine (g/g creatinine); M--the content of trimethyltin chloride in urine (minus the reagent blank) in micrograms (g); V -- the volume of the urine sample taken in milliliters (mL); D--recovery of trimethyltin chloride in urine, %; K--urinary creatinine concentration in grams per liter (g/L).

9 Description

9.1 The detection limit of this method is 0.0025g, the lower limit of quantification is 0.0125g, and the minimum detectable concentration is 0.5g/L (based on 5.0mL of urine sample). The minimum quantitative concentration was 2.5 g/L (based on 5.0 mL of urine sample). The measurement range is from 0.0025μg to 2.5000μg, and the relative standard deviation is 0.6% to 4.4%. 9.2 The average recovery rate of this method is 95.2%. 9.3 This method can use other capillary columns with similar performance. 9.4 Dimethyltin dichloride and methyl tin trichloride coexisting with trimethyltin chloride in urine do not interfere with the determination. 9.5 There is no time limit for urine sample collection. Trimethyltin chloride is slowly and constantly excreted in urine. It can collect random urine from workers. Line detection. 9.6 The quality assurance of the inspection is in accordance with GBZ /T 295. 9.7 Chromatograms and mass spectra are shown in Figures 1 to 3. Note. 1--trimethylethyltin (4.98 min); 2-dimethyldiethyltin (5.98 min); 3--Triethylmethyltin (6.98 min). Figure 1 Separation diagram of trimethyltin chloride derivative, dimethyltin dichloride derivative and methyltin trichloride derivative Figure 2 Mass spectrum of trimethyltin chloride Figure 3 Mass spectrum of trimethyltintin derivative of trimethyltin chloride twenty three ......

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