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HJ 614-2011Soil. Determination of tetramethylene disulphotetramine. Gas chromatography method (English PDF)

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

April 15, 2010

Implementation date

October 1, 2011

Scope

HJ 614-2011 (Soil. Determination of tetramethylene disulphotetramine. Gas chromatography method) is available as an English-translated PDF.

HJ 614-2011 — This standard specifies gas chromatography for the determination of tetramine in soil. This standard applies to the determination of soil poisoning.

When the sample size is 5 g, the detection limit of this method is 3.5 µg/kg, and the lower limit of determination is 14 µg/kg.

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Document preview — HJ 614-2011

National Standard of the People's Republic of China

ICS: 13.080
Classification: Z 18

Issued by: Ministry of Ecology and Environment

Foreword
1 Scope of application
2 Normative references
3 Principle of the method
4 Reagents and materials
5 Instruments and equipment
6 Samples
6.1 Sample collection and preservation
6.2 Preparation of samples
6.3 Preparation of blank samples
6.4 Determination of dry matter content
7 Analysis steps
7.1 Reference chromatographic conditions
7.2 Calibration
7.3 Determination
7.4 Blank test
8 Calculation and representation of results
8.1 Calculation of results
8.2 Results representation
9 Precision and accuracy
9.1 Precision
9.2 Accuracy
10 Quality Assurance and Quality Control
11 Waste treatment

Foreword

In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, protect human health, and standardize the determination method of soil poisoning and rat strength, Develop this standard.

This standard specifies gas chromatography for the determination of tetramine in soil.

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. Changchun Environmental Monitoring Center Station.

This standard is verified by. Shenyang Environmental Monitoring Center Station, Harbin Environmental Monitoring Center Station, Jilin Entry-Exit Inspection and Quarantine Bureau Technology Center, Jilin Province Environmental Monitoring Center Station, Dalian Environmental Monitoring Center and Jilin Province Product Quality Supervision and Inspection Institute.

This standard was approved by the Ministry of Environmental Protection on April 15, 2011.

This standard has been implemented since October 1, 2011.

This standard is explained by the Ministry of Environmental Protection.

Determination of soil tetramine by gas chromatography Warning. The tetramine is a highly toxic substance. The sample preparation process should be carried out in a fume hood. The operator should wear protective equipment to avoid Contact skin and clothing.

1 Scope of application

This standard specifies gas chromatography for the determination of tetramine in soil.

This standard applies to the determination of soil poisoning.

When the sample size is 5 g, the detection limit of this method is 3.5 µg/kg, and the lower limit of determination is 14 µg/kg.

2 Normative references

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

quasi.

HJ 613 Determination of dry matter and moisture in soils - Gravimetric method HJ/T 166 Technical Specifications for Soil Environmental Monitoring

3 Principle of the method

The tetramine in the soil was extracted with ethyl acetate, and the extract was purified and concentrated, separated by gas chromatography, and detected by a nitrogen-phosphorus detector.

Leave time to be qualitative and quantify by external standard method.

4 Reagents and materials

Analytical purification reagents conforming to national standards are used for analysis, unless otherwise stated. The experimental water is freshly prepared distilled water or removed.

Sub-water, chromatographic test without interference peaks.

4.1 Ethyl acetate. excellent grade.

4.2 anhydrous sodium sulfate.

Heat at 300 ° C for 2 h, placed in a desiccator and stored for cooling.

4.3 Tetramine standard stock solution. rho=200 mg/L, directly purchase certified standard solution.

4.4 Standard test solution for tetramine. rho=20 mg/L.

Accurately measure 1.0 ml of tetramine strong standard stock solution (4.3) into a 10 ml volumetric flask, dilute to volume with ethyl acetate (4.1), and mix.

4.5 Quartz sand. 30 ~ 60 mesh, heated at 300 ° C for 2 h before use.

4.6 Glass wool.

After washing with water, it was dried at 105 ° C, washed with ethyl acetate (4.1), dried, and placed in a desiccator for cooling and storage.

4.7 Activated carbon. 30-50 mesh, activated at 300 °C for 2 h before use, placed in a desiccator for cooling and storage.

4.8 High purity nitrogen. purity >= 99.999%.

4.9 High purity hydrogen. purity >= 99.999%.

4.10 High purity air. purity >= 99.999%.

5 Instruments and equipment

5.1 Gas Chromatograph. with nitrogen and phosphorus detector.

5.2 Column 1. 30 m × 0.25 mm, film thickness 0.25 µm, 5% phenyl 95% methylpolysiloxane capillary column. Or other equivalent capillary Column.

5.3 Column 2. 30 m × 0.25 mm, film thickness 0.25 µm, 35% phenyl 65% methylpolysiloxane capillary column. Or other equivalent capillary Column.

5.4 Soxhlet extractor. 250 ml.

5.5 Nitrogen blowing instrument..200 ml with nitrogen blowing tube.

5.6 Glass purification column. hollow glass column with a length of about 10 cm and an inner diameter of 1.2 cm. Fill a small layer of glass wool (4.6) on the bottom of the hollow glass column.

Add 2 g of anhydrous sodium sulfate (4.2), 1.0 g of activated carbon (4.7) and 2 g of anhydrous sodium sulfate (4.2), using 10 ml of ethyl acetate (4.1) Pre-rinse and discard the eluent. A schematic diagram of the glass purification column is shown in Figure 1.

Anhydrous sodium sulfate Activated carbon Glass wool Anhydrous sodium sulfate

Figure 1 purification device diagram

5.7 Analytical balance. Accuracy is 0.01 g.

5.8 separatory funnel. 150 ml.

5.9 Vial. 2 ml, screw glass.

5.10 Quantitative filter paper. phi = 150 mm.

5.11 Microinjectors. 5 µl, 50 µl, 500 µl.

5.12 Common instruments and equipment used in general laboratories.

6 Samples

6.1 Sample collection and preservation

Sample collection was performed in accordance with the relevant regulations of HJ/T 166. Stored at 4 ° C or less and stored within 14 days.

6.2 Preparation of samples

Place the sample on an enamel plate or stainless steel plate to remove debris such as gravel and plant roots and mix well. Weigh 5 g (accurate to 0.01 g) Soil sample, add equal weight of anhydrous sodium sulfate (4.2), and mix well. Wrap it in filter paper and put it in the Soxhlet extractor.

Add 100 ml of ethyl acetate (4.1). The temperature of the water bath was 85-90 ° C, and it was extracted by refluxing 4 times/h for 12-16 h. Transfer the extract to the Soxhlet extractor was washed twice with 20 ml of ethyl acetate (4.1) in a 150 ml separatory funnel and combined with the extract.

Note 1. Extraction methods such as automatic Soxhlet extraction or pressurized solvent extraction can also be used if the recovery rate is met.

Install a purification device (see Figure 1), control the flow rate of 4 ~ 6 ml/min, and collect the eluent with a stoppered triangular flask. With 10 m1 acetic acid the ester (4.1) was cleaned on a glass chromatography column and the eluents were combined. The above eluate was transferred to a.200 ml nitrogen blow tube at a water bath temperature of 60 ° C.

High-purity nitrogen (4.8) was purged and concentrated to about 0.5 ml. The nitrogen purge tube was washed with a small amount of ethyl acetate (4.1) and then treated with ethyl acetate (4.1).

Capacitance to 1.0 ml, then transferred to a 2 ml screw glass vial, sealed, to be tested.

Note 2. Concentration methods such as KD concentrator or rotary evaporation can also be used if the recovery rate is met.

6.3 Preparation of blank samples

A quartz sample (4.5) was used instead of the sample, and a blank sample was prepared in the same manner as in the preparation of the sample (6.2).

6.4 Determination of dry matter content

Accurately weigh a certain amount of fresh soil samples, and determine the dry matter content according to HJ 613.

7 Analysis steps

7.1 Reference chromatographic conditions

Column 1; column temperature. initial temperature 120 ° C for 3 min, 10/min ° C rose to 260 ° C, held for 5 min; gasification chamber and detector Temperature. 280 ° C; carrier gas. high purity nitrogen, column flow. 1.5 ml/min; gas. high purity hydrogen, 3 ml/min; combustion gas. high purity air, 150 ml/min; current intensity. 2 pA; injection method. no splitting; injection volume. 1.0 µl.

7.2 Calibration

Use a micro-syringe to remove 0, 5, 25, 50, 100, and 250 µl of tetramine standard solution (4.4) to 6 1 ml volumetric flasks.

Dilute to the mark with ethyl acetate (4.1) and mix. The standard series concentrations are 0, 0.1, 0.5, 1.0, 2.0, and 5.0 mg/L, respectively.

The analysis was then carried out in order from the low concentration to the high concentration according to the reference chromatographic conditions (7.1). Mass concentration by peak height or peak area (mg/L) is the abscissa and a calibration curve is drawn. The calibration curve correlation coefficient r >= 0.995. The standard chromatogram of tetramine is shown in Figure 2.

9 10 11 12 13 14

1-Poisonous rat, retention time. 13.05 min

Figure 2 Tetramine Strong Standard Chromatogram

7.3 Determination

Measure 1.0 µl of the sample (6.2) into the gas chromatograph and measure according to the reference chromatographic conditions (7.1) to record the retention of the chromatographic peak.

Time and peak height (or peak area).

7.3.1 Qualitative analysis

According to the standard chromatogram, the retention time of the tetramine is qualitative. For samples that can detect tetramine, the reference chromatographic conditions (7.1) should be followed.

Use column 2 for qualitative reanalysis to avoid false positives.

7.3.2 Quantitative analysis

The external concentration method was used to quantitatively calculate the concentration of tetramine in the sample.

7.4 Blank test

A 1.0 µl blank sample (6.3) was weighed into a gas chromatograph and measured according to the reference chromatographic conditions (7.1).

8 Calculation and representation of results

8.1 Calculation of results

The tetramine in the soil sample has a strong content of w (µg/kg), which is calculated according to formula (1).

1 000Vw

rho ×= ×× (1)

Where. w--the content of the poisonous rat in the soil sample, µg/kg;

rho--the strong concentration of tetramine found in the standard curve, mg/L;

V--the volume of the volume of the extract after purification and concentration, ml;

M--sample amount, g;

Wdm - dry matter content (mass fraction), %.

8.2 Results representation

When the measurement result is less than 100 µg/kg, one decimal place is retained, and when the measurement result is greater than or equal to 100 µg/kg, three valid positions are retained.

digital.

9 Precision and accuracy

9.1 Precision

Six laboratory-acquired blank spiked samples of 10 µg/kg,.200 µg/kg, and 400 µg/kg were measured in the laboratory.

The quasi-bias are. 8.1% to 10.9%, 1.7% to 5.2%, 2.3% to 4.7%; the relative standard deviations between laboratories are. 9.7%, 2.2%, 3.1%;

The repeatability limits were. 2.2 µg/kg, 18.2 µg/kg, 34.2 µg/kg; the reproducibility limits were. 3.0 µg/kg, 19.7 µg/kg, 43.9 µg/kg.

9.2 Accuracy

The blanks of 1.0 µg, 2.0 µg and 3.0 µg were measured in 6 laboratories. The recoveries were 83.0%~ 88.0%, 84.8% to 93.2%, 85.9% to 94.6%; the final recovery values were. 85.3% ± 3.6%, 88.5% ± 5.6%, 89.2% ± 7.8%.

The actual samples were spiked and analyzed by 6 laboratories. The standard addition amount was 2.0 µg, and the standard addition recovery rate was 83.0%~87.5%.

The final yield was 85.0% ± 4.0%.

10 Quality Assurance and Quality Control

10.1 At least one blank test shall be performed for each batch of samples, and the results shall be lower than the method detection limit.

10.2 For every 10 samples, analyze the intermediate point concentration standard solution of a calibration curve, and the measurement result is the same as the latest calibration curve.

The relative deviation of the concentration should be less than or equal to 20%.

10.3 At least 10% of parallel samples should be measured for each batch of samples. When the number of samples is less than 10, at least one parallel sample should be measured, twice.

The relative deviation of the parallel determination results should be less than or equal to 20%.

10.4 At least 10% of the spiked samples shall be determined for each batch of samples. When the number of samples is less than 10, at least one spiked sample shall be determined and spiked.

The recovery rate should be between 70% and 120%.

11 Waste treatment

Tetramine is a highly toxic chemical. After the experiment, the equipment used in the experiment is washed with ethyl acetate, and the experiment is produced.

The waste liquid should be stored in a closed container and entrusted to the relevant unit for processing.

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 8 pages — is available in the English PDF.

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