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HJ 896-2017 English PDF

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HJ 896-2017: Water quality. Determination of butyl xanthate. Purge and trap/gas chromatography-mass spectrometry
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Basic data

Standard ID HJ 896-2017 (HJ896-2017)
Description (Translated English) Water quality. Determination of butyl xanthate. Purge and trap/gas chromatography-mass spectrometry
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Classification of International Standard 13.060
Word Count Estimation 11,135
Date of Issue 2017-12-21
Date of Implementation 2018-02-01
Quoted Standard HJ/T 91; HJ/T 164
Regulation (derived from) Ministry of Environmental Protection Announcement 2017 No. 77
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies purge-and-trap/gas chromatography-mass spectrometry for the determination of butyl xanthogen in water. This standard is applicable to the determination of butyl xanthogen in surface water, groundwater, domestic sewage and industrial waste water. This standard does not apply to high-salt industrial wastewater with a salinity higher than 25 g/L, and the presence of water samples such as zeocin (manganese) pesticides or diethyl dithiocarbamate (such as copper reagents). Determination. If butyl xanthate is detected in the water sample, further analysis may be used to confirm further if necessary. When the sample volume was 5 ml, the detection limit of butylxanthogen was 0.04 ��g/L and the lower limit of determination was 0.16 ��g/L.

HJ 896-2017: Water quality. Determination of butyl xanthate. Purge and trap/gas chromatography-mass spectrometry


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(Water quality - Determination of butyl xanthic acid - Purge and trap/gas chromatography - mass spectrometry) People's Republic of China national environmental protection standards Water quality Determination of butyl xanthic acid Purge trap / Gas chromatography - mass spectrometry Water quality-Determination of butyl xanthate-Purge and trap / gas chromatography-mass spectrometry 2017-12-21 Published 2018-02-01 implementation Release MEP i directory Foreword ..ii 1 Scope 1 2 Normative references 1 3 method principle 1 4 interference and elimination .1 5 Reagents and materials .1

6 instruments and equipment

7 samples .3 8 Analysis Step 3 9 results calculated and said 5 Precision and accuracy 11 Quality Control and Quality Assurance 8 12 Waste treatment .8 13 Matters needing attention .8

Foreword

In order to carry out "Law of the People's Republic of China on Environmental Protection" and "Water Pollution Prevention and Control Law of the People's Republic of China", protect the environment and protect people Body health, regulate the determination of butyl xanthic acid in water, the development of this standard. This standard specifies the determination of butyl xanthate in water by purge trap/gas chromatography - mass spectrometry. This standard is released for the first time. This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop. This standard was drafted. China Environmental Monitoring Station. This standard verification unit. Beijing Environmental Protection Monitoring Center, Environmental Monitoring Center of Hebei Province, Zhejiang Province Environmental Monitoring Center, heavy Qing City Ecological Environment Monitoring Center, Ningbo City Environmental Monitoring Center and Yangzhou City Environmental Monitoring Center Station. This standard MEP approved on December 21,.2017. This standard since February 1,.2018 implementation. This standard is interpreted by the MEP. Water quality - Determination of Butyl Xanthic Acid - Purge and Trap/Gas Chromatography - Mass Spectrometry

1 scope of application

This standard specifies the determination of butyl xanthate in water by purge trap/gas chromatography - mass spectrometry. This standard applies to the determination of butyl xanthogen in surface water, groundwater, domestic sewage and industrial wastewater. This standard does not apply to salts containing more than 25 g/L of high salt industrial wastewater and the presence of dexamethasone (manganese) pesticides or diethyl disulfide Substitution of carbamates (eg copper reagents) and other substances in water samples. If the water samples were detected butyl xanthic acid, if necessary, can be used to further confirm other analytical methods. When the sample volume was 5 ml, the detection limit of butyl xanthogen was 0.04 g/L, and the lower limit of determination was 0.16 g/L.

2 Normative references

This standard references the following documents in the terms. For undated references, the effective version applies to this standard. HJ/T 91 Technical Specifications for Surface Water and Sewerage Monitoring HJ/T 164 Groundwater Environmental Monitoring Technical Specifications

3 method principle

Butyl xanthogen in water decomposes under acidic conditions to produce carbon disulfide (CS2), which is indirectly determined by the determination of CS2 Acid concentration. CS2 is purged with high-purity helium (or nitrogen) and adsorbed into the trap. The trap is quickly heated and purged with high-purity helium (or nitrogen Gas) backflushing, the CS2 that is thermally desorbed is separated by gas chromatography and detected with a mass spectrometer. Through the standard solution with butyl xanthogen The retention time and mass spectra of liquid reaction generated CS2 were compared qualitatively with internal standard method.

4 interference and eliminate

The presence of CS2 in the water sample can interfere with the assay and can be subtracted from the difference between the measured values before and after the addition of the acid. The presence of oxidizing substances in the water sample will make the determination result is low, may be appropriate to add 5 ~ 20 mg sodium thiosulfate removal.

5 Reagents and materials

Unless otherwise specified, the analysis of the use of analytical standards in line with national standards of chemical reagents, experimental water for the target does not contain pure water. 5.1 methanol (CH3OH). Chromatography pure. 5.2 concentrated phosphoric acid (H3PO4).  = 1.69 g/ml. 5.3 Sodium hydroxide (NaOH). 5.4 Sodium thiosulfate (Na2S2O3 · 5H2O). 25.5 Potassium butylxanthate (C4H9OCSSK). Purity ≥95%. 5.6 phosphoric acid solution. 1 6. 5.7 Sodium hydroxide solution.  (NaOH) = 400 g/L. Weigh 10 g of sodium hydroxide (5.3) and dissolve to 25 ml with water. 5.8 Sodium hydroxide solution.  (NaOH) = 40 g/L. The sodium hydroxide solution is diluted with water (5.7). 5.9 Sodium hydroxide solution.  (NaOH) = 0.08 g/L. Take.200 l sodium hydroxide solution (5.7) was added to 1L of water. 5.10 butyl xanthic acid standard stock solution.  (C4H9OCSSH) = 100 g/ml. Accurately weigh 0.0330 g potassium butylxanthate (5.5), dissolve in a small amount of water and add 100 l sodium hydroxide solution (5.7), and dilute with water To 250 ml, about 4  C refrigerated, stable for two weeks. 5.11 butyl xanthic acid standard solution.  (C4H9OCSSH) = 10.0 g/ml. With sodium hydroxide solution (5.9) accurate dilution of butyl xanthic acid standard stock solution (5.10), with the current service. 5.12 butyl xanthate standard solution.  (C4H9OCSSH) = 1.00 g/ml. With sodium hydroxide solution (5.9) accurate dilution of butyl xanthic acid standard solution (5.11), with the current available. 5.13 Internal standard solution. fluorobenzene,  = 100 g/ml, the solvent is methanol, a certified standard solution on the market. 5.14 Internal standard solution. fluorobenzene,  = 10.0 g/ml. Use methanol (5.1) to accurately dilute the internal standard solution (5.13). 5.15 Helium. Purity ≥99.999%. 5.16 Nitrogen. Purity ≥99.999%.

6 instruments and equipment

6.1 Gas Chromatography - Mass Spectrometer. The gas chromatograph section has a split/splitless inlet that can be programmed to temperature and the mass spectrometer EI source. 6.2 Purge and Trap. with autosampler and 5 ml purge. Trap tube using 1/3Tenax, 1/3 silica gel, 1/3 activated carbon mixed Adsorbent or other equivalent adsorbent. 6.3 Column. Quartz capillary column with a column length of 60 m, an inner diameter of 0.20 mm, a membrane thickness of 1.12 μm and a stationary phase of 6% cyanopropylidene/94% Dimethylpolysiloxanes, or other equivalent capillary columns. 6.4 Vials. 40 ml brown glass bottle, screw cap with Teflon coated gaskets. 6.5 Volumetric bottles. brown, 50 ml and 250 ml. 6.6 Syringes. 20 l, 100 l and 500 l, with acid-resistant polytetrafluoroethylene piston. 36.7 General laboratory equipment and equipment.

7 samples

7.1 sample collection Collect samples according to HJ/T 91 and HJ/T 164, with a minimum of two bottles per sample. When collecting the sample, slowly introduce the sample into the sample bottle (6.4). Near the full bottle, add the sodium hydroxide solution (5.8) so that the sample The pH is around 10 and finally filled. 7.2 Sample preservation After about 4 C sample collection refrigeration, dark storage and transport, 1d analysis is completed. If not timely analysis, should be added 5 ~ 20 mg Sodium thiosulfate (5.4), about 4 C refrigerated, dark conditions can be stored for two weeks. Sample storage area should be free of carbon disulfide interference.

8 Analysis steps

8.1 Instrument reference conditions 8.1.1 Purge and trapping conditions Sample volume. 5 ml; Purge temperature. 40 ° C; Purge flow rate. 40 ml/min; Purge time. 11 min; Desorption temperature. 180 ° C; Desorption time. 1 min; baking temperature. 190  C; baking time. 10 min; other parameters refer to the instrument user manual to set. 8.1.2 GC analysis conditions Program temperature. 40  C for 1.0 min, with 5  C/min rose to 120  C, hold 1.0 min, and then 20  C/min rose to 250  C, Hold for 2.0 min; Inlet temperature. 230 ° C; Carrier gas flow. 1.0 ml/min; Injection mode. Split injection (split ratio 10.1). 8.1.3 Mass Spectrometry Conditions Electron impact source. EI source; Ionization energy. 70 eV; Ion source temperature. 230 ° C; Transmission line temperature. 280 ° C; Scanning mode Scanning range. 30-300 amu; Quadrupole temperature. 150 ° C; Solvent delay time. 6 min; Other parameters reference instrument User's Manual for setting. Note. In order to increase the sensitivity, the method of selective ion scan can also be used for analysis. For the characteristic ion selection, refer to 9.2. 8.2 Calibration curve drawing reference method Pipette a certain amount of butyl xanthate standard solution (5.11,5.12), were added to the sodium hydroxide solution (5.9) of the 50 ml Volumetric flask (6.5), the preparation of low and high concentrations of two standard series, with sodium hydroxide solution (5.9) volume. Low concentrations of the test target water samples selected low concentration standard series, followed by the concentration of 0.20  g/L, 1.00  g/L, 2.00  g/L, 10.0 g/L, 20.0 g/L, the volume of butyl xanthogen standard solution (5.12) is 0.01 ml, 0.05 ml, 0.10 ml, 0.50 ml, 1.00 ml; high concentration of the test target concentration of water samples selected standard series, the concentration of 10.0  g/L, 50.0  g/L, 100 g/L,.200 g/L, 500 g/L, the amount of butyl xanthogen standard solution (5.11) volume of 0.05 ml, 0.25 ml, 0.50 ml, 41.00 ml, 2.50 ml. Transfer the standard series to a 40 ml sample vial (6.4), fill up and seal, remove.200 l with needle (6.6), then inject Needle (6.6) plus 20  l internal standard solution (5.14), so that the internal standard concentration of 5  g/L, and finally with the needle (6.6) quickly added to 100 l phosphoric acid solution (5.6). According to the instrument reference conditions (8.1), from low concentration to high concentration followed by determination, record CS2 and fluorobenzene retention Time and quantitative ion response. Note. It is also possible to automatically add an internal standard to the autosampler according to the autosampler operating instructions. Under the reference instrument conditions of this standard, the total ion chromatogram of the target compound is shown in Figure 1. Figure 1 Total ion current plot of target compounds 8.2.1 Average relative response factor method The relative response factor (RRFi) of butyl xanthogen in point i of the standard series was calculated according to equation (1). i IS ISi i RRF   (1) Where. RRF - The relative response factor for the CS2 point i in the standard series; - the standard series of points i CS2 response value; ISi - standard series of i-point internal standard response value; IS - standard series of internal standard concentration, μg/L; - Standard Series i point butyl xanthic acid concentration, μg/L. Butyl xanthic average relative response factor RRF, calculated according to equation (2). RRF RRF i  1 (2) 5 Where. RRF - butyl xanthic acid average relative response factor; RRFi - the relative response factor for CS2 at point i in the standard series; n - standard series of points. The standard deviation of the RRF is calculated according to equation (3).       RRFRRF SD (3) Where. SD - standard deviation of RRF; RRF - average relative response of butyl xanthogen; RRFi - the relative response factor for CS2 at point i in the standard series; n - standard series of points. The relative standard deviation of RRF is calculated according to equation (4). 0 RRF SD RSD (4) Where. RSD - relative standard deviation ofRFF; SD - Standard deviation of RFF; RRF - average relative response of butyl xanthogen. 8.2.2 Calibration curve method If the Relative Standard Deviation (RSD) 若20% of the relative response factor (RRF) of butyl xanthogenate is used, calibration curves are required Line calibration. To butyl xanthic acid concentration as abscissa, CS2 response value and the ratio of internal standard response value for the vertical axis, the calibration curve line. 8.3 Determination All samples should be equilibrated to room temperature and then measured. Samples and add internal standards according to standard solution pre-treatment procedure (8.2) to each aliquot One of the bottles of the product is added with 100 l of phosphoric acid solution (5.6) and the other bottle is filled with 100 l of water according to the instrument reference conditions (8.1) 8.2 calibration curve was measured. Note 1. Determination of higher concentrations of butyl xanthic acid water samples, it is recommended diluted with sodium hydroxide solution (5.9) after the determination. Note 2. For strong alkaline wastewater (water sample bottom pH > 10), the volume or concentration of phosphoric acid solution (5.6) can be appropriately increased according to the actual situation. 8.4 Blank test Replace the sample with sodium hydroxide solution (5.9) and perform the blank test according to the same measurement procedure (8.3) as the sample.

9 results calculated and expressed

9.1 The nature of the target 6 According to the sample of butyl xanthogen acid generated by the reaction of carbon disulfide retention time, mass spectrometry, fragment ion mass ratio and its abundance Degree and other information and standard solution after qualitative comparison. The calibration solution should be analyzed more than once to obtain the mean retention time of the target, on average The standard deviation of ± 3 times the retention time is the retention time window, and the retention time of the target in the sample should be within its range. All ions with a relative abundance higher than 10% in the target standard spectrum should exist in the sample spectrum, and the sample mass spectrum and standard The relative abundance deviation of the above characteristic ions in the mass spectrum should be within ± 30%. 9.2 Target quantification After the qualitative identification of the target compound, according to the quantitative ion response value, calculated by internal standard method. Quantitative ions and auxiliary target Ions see Table 1. Table 1 list of target and internal standard ions and auxiliary ions Target Name Type Quantitative ion-assisted ion Carbon disulfide target 76 32,44 Fluorobenzene internal standard 96 70 9.2.1 Quantify with the average relative response factor When the target compound is calculated using the average relative response factor, the mass concentration of butyl xanthogenate in the sample According to formula (5) Calculation. (5) Where.  - sample mass concentration of butyl xanthic acid, μg/L; - Response value of quantitative ion of acid sample CS2; ISx - Acidic sample internal standard quantitative ion response value; - The response of the CS2 ion without the acid sample; ISo - The response of internal standard ion quantification without acid; IS - Internal standard mass concentration, μg/L; f - dilution factor RRF - average relative response of butyl xanthogen. 9.2.2 Quantitative calibration curve When the target compound is quantified using a calibration curve, the mass concentration of butyl xanthogenate in the sample Calculate according to formula (6). 7 (6) Where.  - sample mass concentration of butyl xanthic acid, μg/L; - Response value of quantitative ion of acid sample CS2; ISx - Acidic sample internal standard quantitative ion response value; - The response of the CS2 ion without the acid sample; ISo - The response of internal standard ion quantification without acid; b - calibration curve intercept; f - dilution factor a - calibration curve slope. 9.3 results show When the measurement result < 1 g/L, keep 2 digits after the decimal point. When the measurement result is ≥1 g/L, keep 3 significant digits. 10 precision and accuracy 10.1 Precision Six laboratories had a uniform sample of butyl xanthic acid at concentrations of 1.00 μg/L, 20.0 μg/L and 400 μg/L. The experiments The relative standard deviations (RSDs) were 3.3% ~ 8.4%, 1.9% ~ 5.6%, 0.7% ~ 3.7% respectively. The relative standard deviations 5.6%, 3.6% and 1.9% respectively. The repeatability limits were 0.17 μg/L, 2.2 μg/L and 18 μg/L respectively. The reproducibility limits were 0.29 μg/L, 4.3 μg/L, 50 μg/L. In six laboratories, the surface water samples with the concentration of butylxanthogenic acid of 1.00 μg/L and 5.00 μg/L were tested for precision. The laboratory The relative standard deviations (RSDs) were 1.6% -14% and 1.0% -7.2% respectively. The relative standard deviations (RSDs) were 12% and 10% The limits of detection were 0.30 μg/L and 0.59 μg/L, respectively. The reproducibility limits were 0.41 μg/L and 1.3 μg/L, respectively. In six laboratories, the groundwater samples with the concentrations of butylxanthogenate of 1.00 μg/L and 5.00 μg/L were tested for precision. The laboratory The relative standard deviations were 3.0% ~ 11% and 1.7% ~ 6.8% respectively. The relative standard deviations (RSDs) were 7.1% and 5.5% The limits of detection were 0.18 μg/L and 0.51 μg/L, respectively. The reproducibility limits were 0.23 μg/L and 0.78 μg/L, respectively. The precision of domestic or industrial wastewater samples spiked with butyl xanthic acid at concentrations of 10.0 μg/L and 100 μg/L in 6 laboratories The relative standard deviations (RSDs) in laboratory were 1.4% -18% and 2.0% -7.8% respectively. The relative standard deviations (RSDs) were 9.5% 8.9% respectively. The reproducibility limits were 2.4 μg/L and 14 μg/L, respectively. The reproducibility limits were 3.1 μg/L and 24 μg/L, respectively. 810.2 Accuracy In the six laboratories, the surface water samples with the concentration of butyl xanthogenate of 1.00 g/L and 5.00 g/L were spiked and analyzed. The spiked recoveries were 88.5% -122% and 76.2% -99.1%, respectively. The final spiked recoveries were 103% 25.2% and 90.8% 19.0%. In the six laboratories, groundwater samples spiked with butyl xanthogenate at a concentration of 1.00 g/L and 5.00 g/L were subjected to spike analysis. The spiked recoveries were 90.7% -107% and 91.4% -105%, respectively. The final recoveries were 97.2% 14.0% and 96.6% 10.4%. Six laboratories on the butyl xanthate spiked concentration of 10.0 g/L, 100 g/L of domestic wastewater or industrial wastewater samples were added The standard recoveries were 79.2% -104% and 78.9% -104%, respectively. The final recoveries were 96.8% and 18.2%, respectively. 95.2% 17.0%. 11 Quality control and quality assurance 11.1 Calibration The calibration curve requires a minimum of 5 concentration series. The initial calibration curve should have a correlation coefficient ≥0.995 or relative response factor (RRF) The relative standard deviation should be ≤20%, otherwise, find out the reason or redraw the calibration curve. Every 24 h analysis of the calibration curve of the intermediate concentration point, the measured results and the actual concentration value of the relative deviation should be ≤ 20%, otherwise should Find the cause or redraw the calibration curve. 11.2 Blank test. A blank sample analysis shall be performed for each batch of samples (≤20 pcs.). The content of the target in the blank sample should be low The limit of detection of the method, or should identify the cause, re-analysis until the requirements are met before measuring the sample. 11.3 Determination of parallel samples. Each batch of samples (≤ 20/batch) should be measured at least 5% of the parallel sample, the sample number is less than 20, At least one parallel sample should be determined. The relative deviation of the results of parallel samples should be ≤ 30%. Note. The sample in each vial can only be analyzed once the specificity of butyl xanthate has been determined. 11.4 Determination of spiked samples. Each batch of samples (≤ 20/batch) should be measured at least one matrix spiked samples, the spike recovery in 70.0% ~ 130%. 12 Waste treatment The waste liquid generated in the experiment should be collected in a centralized manner and properly stored, entrusted to a qualified unit for handling. 13 Precautions 13.1 Reaction Products CS2 Volatile, need to use a good seal of the sample bottle. 13.2 In the process of experimental operation, the needle, purge pipe and other long-term in the acid system conditions easily corroded, it is recommended to add acid and not added Acid sample cross-test, and after the test is completed thoroughly washed with water injection system. 13.3 The reaction acid can also be used 1 1 hydrochloric acid, but because of its strong volatility, special attention to the purge line after the test cleaning. 13.4 If the spiked recoveries of the sample matrix are less than 70% after many determinations, consider the alkalinity of the water sample is too large or the salt content is higher than 25g/L.

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