|
US$119.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
GBZT312-2018: Determination of N-methyl acetamide in urine -- Gas chromatography method
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GBZ/T 312-2018 | English | 119 |
Add to Cart
|
3 days [Need to translate]
|
Determination of N-methyl acetamide in urine -- Gas chromatography method
| Valid |
GBZ/T 312-2018
|
PDF similar to GBZT312-2018
Standard similar to GBZT312-2018 GBZ 20 GBZ 57 GBZ 49 GBZ/T 303 GBZ/T 302 Basic data | Standard ID | GBZ/T 312-2018 (GBZ/T312-2018) | | Description (Translated English) | Determination of N-methyl acetamide in urine -- Gas chromatography method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | C60 | | Word Count Estimation | 6,661 | | 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 312-2018: Determination of N-methyl acetamide in urine -- Gas chromatography 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 N-methylacetamide in urine - Gas chromatography method
ICS 13.100
C 52
National Occupational Health Standards
Determination of N-methylacetamide in urine - Gas chromatography
Determination of N-methylacetamide in urine-
Gas chromatographic 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
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was drafted. Zhejiang Academy of Medical Sciences, Zhejiang Provincial Center for Disease Control and Prevention, Guangdong Provincial Hospital for Occupational Diseases, Shanghai
Disease Prevention and Control Center.
The main drafters of this standard. Qian Yaling, Tang Hongfang, Qi Zheng, Wang Wei, Zhu Haibao, Liu Danhua, Wu Banghua, Wen Yimin, Zhao Yongxin.
Determination of N-methylacetamide in urine - Gas chromatography
1 Scope
This standard specifies gas chromatography for the determination of N-methylacetamide in urine.
This standard applies to the determination of N-methylacetamide in the urine of occupational exposure personnel.
2 Normative references
The following documents are indispensable for the application of this document. For dated references, only the dated version applies to this document.
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
After the urine sample (hereinafter referred to as the urine sample) is frozen, centrifuged, and precipitated with methanol, the N-A in the urine is separated by a polar capillary column.
Acetylamine, detected by a nitrogen-phosphorus detector, is characterized by retention time and peak area is quantified.
4 instruments
4.1 Covered polyethylene plastic bottle. 50mL.
4.2 Covered polyethylene plastic centrifuge tube. 5mL, 10mL.
4.3 Centrifuge. 5000r/min.
4.4 Microinjector. 1 μL.
4.5 Gas chromatograph with nitrogen and phosphorus detector, autosampler.
Instrument operation reference conditions.
a) Column. 30 m × 0.53 mm × 1.0 μm bonded/crosslinked polyethylene glycol (PEG-20M);
b) Column temperature. initial temperature 100 ° C, hold for 1 min, raise temperature to 170 ° C at 25 ° C/min, hold for 3 min, heat up to 10 ° C/min to
210 ° C, kept for 3 min;
c) vaporization chamber temperature. 250 ° C;
d) detection chamber temperature. 320 ° C;
e) carrier gas (nitrogen) flow. 6.0 mL/min;
f) Split ratio. 10.1.
5 reagent
5.1 Experimental water. chromatographic identification of interference-free peaks.
5.2 Methanol solution. 80% (volume fraction), chromatographic identification of interference-free peaks.
5.3 Standard solution. Accurately weigh a certain amount of N-methylacetamide (content ≥99%, dissolved in warm water and then take it), diluted with methanol solution
Release and make up to a certain volume, make a standard stock solution, store in a refrigerator at 4 °C, and set aside. When used, it is diluted with methanol solution to a concentration of
Standard application solution 1 at 1.00 mg/mL and standard application solution 2 at a concentration of 0.020 mg/mL.
6 Sample collection, transportation and storage
Cover the polyethylene plastic bottle to collect 50mL of the end of the working hours of occupational exposure to dimethylacetamide workers, and tighten the cap after the chamber
It can be stored in a refrigerator at -18 °C for two weeks.
7 Analysis steps
7.1 Blank inspection. Take 1.0mL water and transfer to a 5mL centrifuge tube, add 4.0mL methanol solution, mix and measure for determination.
No interference peaks.
7.2 Sample processing. After the frozen urine sample is thawed at room temperature, mix it, and take 10 mL of urine into a 10 mL stoppered centrifuge tube to 3000
Centrifuge for 10 min at r/min, accurately absorb 1.0 mL of the supernatant and transfer to a 5 mL stoppered centrifuge tube, add 4.0 mL of methanol solution, mix, and then
Centrifuge for 10 min at 3000 r/min and the supernatant was assayed.
7.3 Standard curve drawing. Accurately add 0.0 mL, 0.10 mL, 0.20 mL, 1.00 mL of standard application solution 2 in a 10 mL volumetric flask.
And 0.10mL, 0.50mL of the standard application solution 1, add water 2.0mL, dilute to the mark with methanol solution, formulated to a concentration of 0.0μg/mL,
N-methylacetamide standard series of 0.20 μg/mL, 0.40 μg/mL, 2.00 μg/mL, 10.0 μg/mL, 50.0 μg/mL; reference instrument operation
Conditions, the gas chromatograph was adjusted to the optimum measurement state, 0.2 μL was injected, and each standard series was measured, and each concentration was repeatedly measured three times.
Qualitative retention time, with the concentration of N-methylacetamide (μg/mL) as the abscissa, the mean value of the peak area measured is plotted on the ordinate.
Curve or calculate regression equations.
7.4 Sample determination. The urine sample supernatant solution is determined by the operating conditions of the assay standard series, and the measured peak area value is determined by a standard curve or
The regression equation was used to obtain the concentration (μg/mL) of N-methylacetamide in the sample solution. If the concentration of N-methylacetamide in the sample exceeds the measurement range
Dilute, can be determined by dilution with methanol solution, multiplied by the dilution factor.
8 calculation
8.1 Calculate the concentration of N-methylacetamide in urine according to formula (1).
C=5C0 (1)
In the formula.
C-- concentration of N-methylacetamide in urine, in milligrams per liter (mg/L);
5-- dilution factor for pretreatment of urine sample;
C0--Measured concentration of N-methylacetamide in the urine sample solution in micrograms per milliliter (μg/mL).
8.2 In order to calibrate the dilution of urine, creatinine should be measured as soon as possible after urinary sample collection according to WS/T 97 or WS/T 98. See formula (2) for the correction formula.
Cr
=m (2)
In the formula.
m--Concentration of N-methylacetamide in urine samples after creatinine correction, in milligrams per gram of creatinine (mg/g creatinine);
C--the concentration of N-methylacetamide in urine, in milligrams per liter (mg/L);
Cr--urinary creatinine concentration in grams per liter (g/L).
9 Description
9.1 The determination range of this method is 0.20μg/mL ~ 50.0 μg/mL, the detection limit is 0.04 μg/mL, and the minimum detection concentration is 0.2 mg/L (to take
1.0 mL of urine sample was adjusted to 5 mL with methanol solution, the relative standard deviation was 1.5%~3.4%, and the recoveries were 96.0%-99.4%.
9.2 If manual injection is performed with a micro-syringe, the final standard series and the urine sample supernatant should be diluted 5 times with methanol solution.
The whole is 1.0 μL.
9.3 After measuring a high concentration of urine sample, if a low concentration urine sample is subsequently measured, it is necessary to apply a methanol solution several times to clean the chromatographic system until
No interference peaks.
9.4 Samples can be stored at -18 ° C for 2 weeks.
9.5 Interference test. When dimethylformamide and dimethylacetamide coexist in the air of the workplace, the metabolite N- in the urine sample of the contact
In addition to methyl acetamide, there are also N-methylformamide, acetamide, formamide, and unconverted dimethylformamide and dimethylacetamide.
The results indicate that the other five amides do not interfere with the determination of N-methylacetamide in the urine. If there is no coexistence of dimethylformamide in the workplace air, ie urine
In the absence of N-methylformamide, a bonded/crosslinked polyethylene glycol (PEG) capillary color of 30 m × 0.32 mm × 0.25 μm can also be used.
Column determination.
9.6 Quality control during the test shall be carried out in accordance with GBZ /T 295.
9.7 The chromatographic separation of the urine sample determination is shown in Figure 1.
Note.
A--dimethylformamide;
B--dimethylacetamide;
c--N-methylacetamide;
d--N-methylformamide;
E--acetamide;
F--formamide.
Figure 1 Chromatographic separation of urine coexisting materials
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GBZT312-2018_English be delivered?Answer: Upon your order, we will start to translate GBZT312-2018_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of GBZT312-2018_English with my colleagues?Answer: Yes. The purchased PDF of GBZT312-2018_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.
|