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HJ 696-2014Water quality. Determination of turpentine. Gas chromatography method (English PDF)

水质松节油的测定气相色谱法

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

March 31, 2014

Implementation date

July 1, 2014

Scope

HJ 696-2014 is the English-translated version of 水质松节油的测定气相色谱法.

HJ 696-2014 — This standard specifies gas chromatography for the determination of turpentine in water. This standard applies to the determination of turpentine in surface water, groundwater, industrial wastewater and domestic sewage.

When the sample amount is 100ml, the detection limit of this standard is 0.03mg/L, and the lower limit of determination is 0.12mg/L.

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Document preview — HJ 696-2014

National Standard of the People's Republic of China

Classification: Z 16

Issued by: Ministry of Ecology and Environment

Foreword
1 Scope of application
2 Normative references
3 Principle of the method
4 Reagents and materials
4.4 Sodium Chloride (NaCl)
4.5 Anhydrous sodium sulfate (Na2SO4)
5 Instruments and equipment
6 Samples
6.1 Sample collection and preservation
6.2 Preparation of samples
6.3 Preparation of blank samples
7 Analysis steps
7.1 Recommended chromatographic conditions
7.2 Drawing a calibration curve
7.3 Determination of samples
7.4 Blank test
8 Calculation and representation of results
8.1 Qualitative analysis
8.2 Quantitative analysis
8.3 Result representation
9 Precision and accuracy
9.1 Precision
9.2 Accuracy
10 Quality Assurance and Quality Control
11 Waste treatment

Foreword

To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on Water Pollution Prevention and Control, to protect the environment, this standard is formulated to ensure human health and standardize the determination method of turpentine in water.

This standard specifies gas chromatography for the determination of turpentine in water.

This standard is the first release.

This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.

This standard is mainly drafted by. Taizhou Environmental Monitoring Center Station.

This standard is verified by. Jiangsu Environmental Monitoring Center, Wuxi Environmental Monitoring Center Station, Suzhou Environmental Monitoring Center Station, Changzhou Environmental Monitoring Center, Zhenjiang Environmental Monitoring Center Station and Taizhou Environmental Monitoring Center Station.

This standard was approved by the Ministry of Environmental Protection on March 31, 2014.

This standard has been implemented since July 1, 2014.

This standard is explained by the Ministry of Environmental Protection.

Water quality turpentine - Determination of gas chromatography Warning. The reagents and standard solutions used in this method are volatile toxic compounds. The preparation process should be in the fume hood.

Carry out; protective equipment should be worn as required to avoid contact with skin and clothing.

1 Scope of application

This standard specifies gas chromatography for the determination of turpentine in water.

This standard applies to the determination of turpentine in surface water, groundwater, industrial wastewater and domestic sewage.

When the sample amount is 100ml, the detection limit of this standard is 0.03mg/L, and the lower limit of determination is 0.12mg/L.

2 Normative references

The contents of this standard refer to the terms in the following documents. For undated references, the valid version applies to this standard.

HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring

3 Principle of the method

The turpentine in the sample is extracted with dichloromethane, and the extract is dehydrated and dried, and the gas phase is detected by a hydrogen flame ionization detector.

The chromatographic test was performed according to the retention time of alpha-pinene and beta-pinene, the main components in turpentine, and quantified by external standard method.

4 Reagents and materials

Analytical purification reagents in accordance with national standards were used for analysis, unless otherwise stated.

Sub-water or distilled water.

4.1 Dichloromethane. pesticide residue level.

4.2 Turpentine standard solution. rho = 20 mg/ml, the solvent is methanol.

4.3 Standard use of turpentine. accurately transfer a certain amount of turpentine standard solution (4.2) with dichloromethane (4.1) A standard use solution with a mass concentration of 1000.0 mg/L was released.

4.4 Sodium Chloride (NaCl)

After burning at 400 ° C for 4 h, it was cooled and placed in a ground glass bottle and stored in a desiccator.

4.5 Anhydrous sodium sulfate (Na2SO4)

After burning at 400 ° C for 4 h, it was cooled and placed in a ground glass bottle and stored in a desiccator.

4.6 Nitrogen. purity >= 99.999%.

4.7 Hydrogen. purity >= 99.95%.

4.8 Gas. Compressed air.

5 Instruments and equipment

5.1 Gas Chromatograph. Hydrogen flame ionization detector.

5.2 Column 1. quartz capillary column, 30m × 0.25mm, coated with 5% phenylmethylpolysiloxane, film thickness 0.25µm, or other equivalent capillary column.

5.3 Column 2. quartz capillary column, 30m × 0.25mm, internally coated with 35% phenylmethylpolysiloxane, film thickness 0.25µm, or other equivalent capillary column.

5.4 Oscillator.

5.5 separatory funnel. 250 ml.

5.6 Microinjectors. 10µl, 100µl, 250µl.

5.7 Drying column. glass column with a length of 250mm and an inner diameter of 20mm, and the glass piston is not coated with lubricating oil. At the lower end of the column, put less A glass wool or glass fiber filter paper was added, and 10 g of anhydrous sodium sulfate (4.5) was added.

5.8 Box type electric furnace.

5.9 Common instruments and equipment used in general laboratories.

6 Samples

6.1 Sample collection and preservation

Samples were taken with reference to the relevant regulations of HJ/T 91 and HJ/T 164.

Samples were taken using a 250 ml hard-ground glass bottle or a brown threaded glass bottle with a Teflon septum. At 4 ° C Store underneath, extract within 48h, and extract for 7d.

6.2 Preparation of samples

Take 100.0 ml of the sample into a 250 ml separatory funnel, add 2.5 g of sodium chloride (4.4), dissolve and add 10.0 ml.

Dichloromethane (4.1), shaken and vented, placed on a shaker and shaken vigorously for 5 min, allowed to stand for 10 min, layered, and collected dichloro the methane extract is dehydrated using a dry column or other type of drying equipment and 1.0 ml is to be tested.

Note. For samples with complex composition, if the emulsification phenomenon is serious during the extraction process, mechanical separation should be used to complete the two-phase separation, including it can be broken by agitating, centrifuging, filtering with glass wool, etc., or it can be broken by freezing.

6.3 Preparation of blank samples

A 100.0 ml portion of distilled water was weighed instead of the sample, and a blank sample was prepared in accordance with the same procedure as in the preparation of the sample (6.2).

7 Analysis steps

7.1 Recommended chromatographic conditions

Inlet temperature. 180 ° C; splitless injection; column flow rate. 1.0 ml/min; oven temperature.

10/ min 30/ min60 min 110 min 230 min----> ---->°C °C(10) °C(1) °C(5); detector temperature. 260°C; sample Product. 1.0 µl.

7.2 Drawing a calibration curve

Take 6 10ml volumetric flasks, add appropriate amount of dichloromethane (4.1), and add 0.0, 10.0 with a micro-syringe.

20.0, 50.0, 100.0, 250.0 µl of turpentine standard use solution (4.3), make up to volume with dichloromethane, and mix. Made into pine the fuel-saving mass concentration is a standard series of 0.0, 1.00, 2.00, 5.00, 10.0, 25.0 mg/L, respectively. Standard solution series the concentration (mg/L) is the abscissa, and the corresponding peak response value (the sum of the peak height or peak area of alpha-pinene and beta-pinene) for the ordinate, draw a calibration curve.

7.3 Determination of samples

1.0 µl of the sample to be tested (6.2) was injected into the gas chromatograph and the measurement was carried out under the same chromatographic conditions as the calibration curve.

Record the retention time and peak area (or peak height) of the chromatographic peak.

7.4 Blank test

While the sample is being analyzed, a blank test should be performed. Take 1.0µl blank sample (6.3) into the gas chromatograph, press

7.3 Determine the same steps for analysis.

8 Calculation and representation of results

8.1 Qualitative analysis

Take a certain amount of turpentine standard solution (4.2), dilute to 25.0 mg/L with dichloromethane (4.1), take 1.0 µl injection, Characterize the retention time of the turpentine chromatographic peak, see Figure 1.

Figure 1 Standard chromatogram of turpentine (column 1)

If the target compound is detected, use column 2 to aid in qualitative confirmation, see Figure 2.

Figure 2 Turpentine-assisted qualitative chromatogram (column 2)

8.2 Quantitative analysis

The mass concentration (mg/L) of turpentine in the sample is calculated according to formula (1).

rhorho = × (1)

In the formula.

rho--the mass concentration of turpentine in the sample, mg/L;

rho1-- Calculate the pine in the sample to be tested from the calibration curve based on the sum of the peak areas (or peak heights) of alpha-pinene and beta-pinene Mass concentration of oil saving, mg/L;

V 1--sample volume, ml;

V2--extract volume, ml.

8.3 Result representation

When the measurement result is less than 1.00 mg/L, it is retained to two decimal places; when the measurement result is greater than or equal to 1.00 mg/L, Keep three significant digits.

9 Precision and accuracy

9.1 Precision

Six laboratories tested the uniform samples with turpentine concentrations of 0.10mg/L, 0.50mg/L, and 1.50mg/L, respectively.

The relative standard deviations in the experimental room were. 6.0%~8.1%, 3.8%~10.1%, 2.8%~5.9%; the relative standard between laboratories the deviations were. 5.7%, 6.6%, 3.9%; the repeatability limits were. 0.02 mg/L, 0.09 mg/L, 0.18 mg/L;

The sexual limits were. 0.03 mg/L, 0.12 mg/L, and 0.23 mg/L, respectively.

9.2 Accuracy

Six laboratories conducted certified standard substances with turpentine concentrations of 0.10 mg/L, 0.50 mg/L, and 1.50 mg/L, respectively.

The relative errors are. -5.6%~7.9%, -8.4%~5.5%, -4.7%~5.8%; the relative error final values are.

-0.58% ± 12.4%, -2.40% ± 11.2%, 1.37% ± 7.3%.

Six laboratories carried out spiked analysis and analysis on surface water, domestic sewage and industrial wastewater samples, respectively.

The recoveries of 0.010mg, 0.050mg and 0.150mg were 83.2%~93.0%, 84.6%~103% and 91.3%~103% respectively.

The final recoveries of the spiked recoveries were 87.6% ± 6.9%, 90.6% ± 13.4%, and 95.0% ± 8.8%, respectively.

10 Quality Assurance and Quality Control

10.1 At least one laboratory blank should be made for each batch of samples, and the blank value should be lower than the method detection limit. Otherwise, the cause should be ascertained.

10.2 The correlation coefficient of the calibration curve should be >=0.995, otherwise the calibration curve should be redrawn.

10.3 Continuous calibration. For every 20 samples measured, a standard solution of the concentration at the midpoint of the calibration curve shall be determined.

The relative error of this point concentration with the calibration curve should be <= 20%. Otherwise, the calibration curve needs to be redrawn.

10.4 At least 10% of parallel samples should be determined for each batch of samples. When the number of samples is less than 10, at least one parallel should be determined.

Double. When the measurement result is within 10 times the detection limit (including the detection limit of 10 times), the relative deviation of the results of the parallel double sample measurement should be <= 50%; when the measurement result is greater than 10 times the detection limit, the relative deviation of the parallel double sample measurement results should be <= 20%.

10.5 At least one spiked sample shall be determined for each batch of samples, and the spiked recovery rate shall be between 70% and 130%.

11 Waste treatment

The organic waste generated by the experiment should be stored in a centralized manner and entrusted to a qualified unit for processing.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 7 pages — is available in the English PDF.

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