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GB/T 5750.10-2006 English PDF (GBT5750.10-2006)

GB/T 5750.10-2006 English PDF (GBT5750.10-2006)

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GB/T 5750.10-2006: Standard examination methods for drinking Water -- Disinfection by-products parameters

This standard specifies the use of headspace gas chromatography for the determination of dichloromethane, 1,1-dichloroethane and 1,2- dichloroethane in drinking water and its source water.
GB/T 5750.10-2006
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 13.060
C 51
Partially replacing GB/T 5750-1985
Standard examination methods for drinking water -
Disinfection by-products parameters
ISSUED ON. DECEMBER 29, 2006
IMPLEMENTED ON. JULY 01, 2007
Issued by. Ministry of Health of the People's Republic of China;
Standardization Administration of the People's Republic of
China.
Table of Contents
1 Trichloromethane .. 6
2 Tribromomethane .. 6
3 Dichloro-bromomethane .. 6
4 Chlorodibromomethane . 6
5 Dichloromethane .. 6
6 Formaldehyde .. 11
7 Acetaldehyde . 15
8 Trichloroacetaldehyde . 21
9 Dichloroacetic acid . 26
10 Trichloroacetic acid .. 31
11 Cyanogen chloride .. 31
12 2,4,6-trichlorophenol .. 33
13 Chlorite .. 44
14 Bromate . 56
Appendix A (Normative) References .. 65
Foreword
GB/T 5750 "Standard Test Method for Drinking Water" is divided into the following parts.
- General principles;
- Collection and preservation of water samples;
- Water analysis quality control;
- Organoleptic and physical parameters;
- Nonmetal parameters;
- Metal parameters;
- Aggregate organic parameters;
- Organic parameters;
- Pesticides parameters;
- Disinfection by-products parameters;
- Disinfectants parameter;
- Microbiological parameters;
- Radiological parameters.
This standard replaces chloroform in the part II of GB/T 5750-1985 ?€?Standard examination methods for drinking water?€?.
As compared with GB/T 5750-1985, the main changes are as follows.
- ADJUST the structure in accordance with GB/T 1.1-2000 ?€?Directives for standardization - Part 1. Rules for the structure and drafting of standards?€? and GB/T 20001.4-2001 ?€?Rules for drafting standards - Part 4. Methods of chemical analysis?€?;
- REVISE the quantity and measurement unit in accordance with the
requirements of national standards;
- CHANGE the equivalent concentration into the molar concentration (the redox part still retains the equivalent concentration);
- CHANGE the mass concentration indication symbol C into ??, CHANGE the
Standard examination methods for drinking water -
Disinfection by-product parameters
1 Trichloromethane
Same as the test method for carbon tetrachloride in Chapter 1 of GB/T 5750.8- 2006.
2 Tribromomethane
Same as the test method for carbon tetrachloride in Chapter 1 of GB/T 5750.8- 2006.
3 Dichloro-bromomethane
Same as the test method for carbon tetrachloride in Chapter 1 of GB/T 5750.8- 2006.
4 Chlorodibromomethane
Same as the test method for carbon tetrachloride in Chapter 1 of GB/T 5750.8- 2006.
5 Dichloromethane
5.1 Headspace gas chromatography
5.1.1 Scope
This standard specifies the use of headspace gas chromatography for the determination of dichloromethane, 1,1-dichloroethane and 1,2-dichloroethane in drinking water and its source water.
This method applies to the determination of dichloromethane, 1,1-
dichloroethane and 1,2-dichloroethane in drinking water and its source water. The minimum detection mass concentration of this method. dichloromethane 9 ??g/L, 1,1-dichloroethane 8 ??g/L, 1,2-dichloroethane 13 ??g/L.
Under the operating conditions of this method, other halogenated hydrocarbons do not interfere.
5.1.2 Principle
In a closed headspace bottle, volatile halogenated hydrocarbon molecules escape from the liquid phase into the gas in the headspace. At a certain temperature, the molecules of the halogenated hydrocarbon reach a dynamic equilibrium between the gas and liquid phases, at this time the concentration of the halogenated hydrocarbon in the gas phase is proportional to its
concentration in the liquid phase. By measuring the concentration of the halogenated hydrocarbon in the gas phase, it can calculate the mass
concentration of the halogenated hydrocarbon in the water sample.
5.1.3 Reagents and materials
5.1.3.1 Carrier gas and auxiliary gas
5.1.3.1.1 Carrier gas. High purity nitrogen (99.999%).
5.1.3.1.2 Gas. Pure hydrogen (> 99.6%).
5.1.3.1.3 Combustion supporting gas. Oil-free compressed air, which is purified by a purge tube containing 0.5 nm molecular sieves.
5.1.3.2 Reagents for preparing standard samples and reagents
5.1.3.2.1 Pure water (fresh deionized water).
5.1.3.2.2 Chromatographic standards (chromatographically pure).
dichloromethane, 1,1-dichloroethane, 1,2-dichloroethane.
5.1.3.3 Reagents and materials for preparing columns
5.1.3.3.1 Columns and fillings are as shown in the relevant contents of 5.1.4.1.3. 5.1.3.3.2 The solvent used for the coating fixative solution. chloroform + butanol (1 + 1).
5.1.4 Instruments
5.1.4.1 Gas chromatograph
5.1.4.1.1 Hydrogen flame ionization detector.
5.1.4.1.2 Logger or workstation.
5.1.4.1.3 Column
40 min, which can be used for analysis after gas-liquid equilibrium.
5.1.6 Analytical procedures
5.1.6.1 Instrument adjustment
5.1.6.1.1 Gasification chamber temperature. 200 ??C.
5.1.6.1.2 Column temperature. 85 ??C.
5.1.6.1.3 Detector temperature. 200 ??C.
5.1.6.1.4 Gas flow. Carrier gas 50 mL/min; hydrogen 52 mL/min; air 700 mL/min. 5.1.6.1.5 Attenuation. ADJUST the recorder attenuation in accordance with the content of the measured component in the sample.
5.1.6.2 Calibration
5.1.6.2.1 Calibration method in quantitative analysis. external standard method. 5.1.6.2.2 Standard samples
A. Number of uses. Each time the sample is analyzed, USE the new standard use solution to draw the standard curve or USE the response factor to make calculation.
B. Preparation of standard samples. TAKE three 10 mL volumetric flasks, ADD a few milliliters of distilled water, accurately WEIGH it, respectively ADD one drop of dichloromethane, 1,1-dichloroethane, and 1,2-dichloroethane.
Accurately WEIGH it, the mass increased is the mass of dichloromethane, 1,1- dichloroethane, and 1,2-dichloroethane. USE pure water to make the volume reach to the mark. After calculating the content, respectively TAKE appropriate amount of this solution, DILUTE it to ?? (dichloromethane) = 5 ??g/mL, ?? (1,1- dichloroethane) = 7.5 ??g/mL, ?? (1, 2-dichloroethane) = 7.5 ??g/mL, PREPARE it before use.
C. Conditions for use of standard solutions in gas chromatography.
a The standard solution injection volume is the same as the specimen
injection volume. When measured by the single standard method, the
standard solution response value shall be close to the specimen response value.
b When the relative standard deviation is less than 10% within the working range, the instrument is considered to be in a stable state.
c Standard samples and specimen are injected for analysis as far as
possible at the same time.
Under selected chromatographic conditions, formaldehyde, propionaldehyde, acetone, and butyraldehyde do not interfere with the determination.
7.1.2 Principle
Acetaldehyde and acrolein in water can be directly separated and measured by gas chromatography with a hydrogen flame ionization detector. The peak order is acrolein and acetaldehyde.
7.1.3 Reagents and materials
7.1.3.1 Carrier gas and auxiliary gas
7.1.3.1.1 Carrier gas. High purity nitrogen (99.999%).
7.1.3.1.2 Combustion gas. Pure hydrogen (> 99.6%).
7.1.3.1.3 Combustion supporting gas. Oil-free compressed air, which is purified by a purge tube fitted with a 0.5 nm molecular sieve.
7.1.3.2 Reagents for preparing standard samples and specimen
pretreatments
7.1.3.2.1 Sodium bisulfite solution [c(NaHSO3) = 0.05 mol/L]
7.1.3.2.2 Iodine standard solution [c (1/2 I2) = 0.10 mol/L], to be calibrated. 7.1.3.2.3 Sodium thiosulfate standard solution [c (Na2S2O3) = 0.10 mol/L], to be calibrated.
7.1.3.2.4 Starch solution (5 g/L).
7.1.3.2.5 Sulfuric acid solution (1 + 1).
7.1.3.2.6 Standard. Acrolein and acetaldehyde solution [??(CH3CHO) = 40%]. 7.1.3.3 Reagents and materials for preparing columns
7.1.3.3.1 Columns and fills are described in 7.1.4.1.3.
7.1.3.3.2 Solvent used for coating fixative. dichloromethane.
7.1.4 Instruments
7.1.4.1 Gas chromatograph
7.1.4.1.1 Hydrogen flame ionization detector.
7.1.4.1.2 Logger or workstation.
DRY it naturally, PREPARE for use.
8.1.4.5 PTFE membrane or aluminum foil.
8.1.4.6 Constant temperature water bath. Control temperature ?? 1 ??C.
8.1.5 Samples
8.1.5.1 Sampling method and storage method. TAKE two headspace bottles
containing 0.1 g of sodium thiosulfate to the site, FILL it with water samples, immediately USE overturn rubber plugs which are wrapped with aluminum foil (or PTFE membrane) to seal it, BRING it back to the laboratory. If it cannot be determined immediately, it must be kept in the refrigerator.
8.1.5.2 Water sample pretreatment. After the water sample is sent to the laboratory, POUR some water sample in the environment without chloroform to make the water sample in the bottle to 50 mL mark, immediately COVER the bottle stopper. PLACE one bottle directly in a constant temperature water bath at 40 ??C as the bottle l, USE the injection needle to inject 0.2 mL of sodium hydroxide solution (8.1.3.2.2) into another bottle, SHAKE it uniformly, PLACE it into a constant temperature water bath at 40 ??C as a bottle II, both of which are equilibrated in a 40 ??C water bath for 2.5 h.
8.1.6 Analytical procedures
8.1.6.1 Instrument adjustment
8.1.6.1.1 Gasification chamber temperature. 200 ??C.
8.1.6.1.2 Column chamber temperature. 150 ??C.
8.1.6.1.3 Detector temperature. 250 ??C.
8.1.6.1.4 Carrier gas flow. 80 mL/min.
8.1.6.2 Calibration
8.1.6.2.1 Calibration method in quantitative analysis. external standard method. 8.1.6.2.2 Standard samples
A. Number of uses. Each time the sample is analyzed, USE the newly prepared standard use solution.
B. Preparation of standard samples
a. Preparation of standard stock s...

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