Determination of 37 Volatile Organic Compounds/35 Volatile Halogenated Hydrocarbons in Solid Waste Headspace/Gas Chromatography-Mass Spectrometry (2)

Six, analysis and testing

(1) Instrument conditions (for reference only, can be adjusted appropriately according to the actual instrument)

1.

Sample bottle standby flow rate: 20mL/min

Heating box temperature: 75℃

Quantitative loop temperature: 100℃

Transmission line temperature: 110℃

Sample bottle balance: 20min (solid waste extract)/30min (solid waste)

Injection duration: 0.

GC cycle time: 42min

Sample bottle volume: 20mL

Vial shaking: Level 5, 71 times/min, acceleration at 260cm/s³

Filling pressure: 15psi

2.

Injection port: temperature is 250℃, column flow rate is 1.

3.

EI ion source, temperature 250℃, ionization energy 70eV; SIM scan parameters are shown in Table 4-1

Table 4-1 SIM scan parameters

According to the performance of the instrument and the relevant standard limit requirements, the data can also be collected in a full scan mode.
The full scan parameter is 35 ~ 280 amu
.
The grouping situation can be adjusted according to the separation of each peak and the number of description points of each peak (usually more than 10)
.

The above SIM scan parameters are also applicable to the data collection of the factors listed in HJ.
642-2013, HJ 643-2013, HJ 714-2014 and HJ736 -2015
.

(2) Retention time and standard curve

1.
Leachate

Add 10 mL leaching solution to the headspace bottle, and prepare a standard series of more than 5 points (such as 5.
00ug/L, 10.
0ug/L, 40.
0ug/L, 70.
0ug) that meets the instrument's detection limit, linear range and actual sample mass concentration.
/L, 100ug/L), add the same amount of internal standard and substitute (such as 50ug/L) of the same product, and quantify with the internal standard method to obtain a binary linear regression curve or average relative correction factor for each compound
.
The retention time, qualitative and quantitative reference ions of each compound under the reference instrument conditions are shown in Table 4-2
.

Table 4-2 37 kinds of volatile organic compounds retention time and qualitative, fixed reference ions

2.
Solid waste

Add 2g of pure quartz sand and 10mL matrix modifier to the headspace bottle, and then take an appropriate amount of standard solution in the above headspace bottle to prepare a standard series of more than 5 points that meets the detection limit of the instrument, the linear range and the actual sample mass concentration (Such as 5.
00ug/L, 10.
0ug/L, 40.
0ug/L, 70.
0ug/L, 100ug/L), add the same amount of internal standard substance and substitute (such as 50ug/L), internal standard method Quantitative
.

The compound retention time, qualitative and quantitative reference ions obtained under the conditions of the reference instrument are shown in Table 4-3
.

Table 4-3 Retention time and qualitative and quantitative reference ions of 35 volatile halogenated hydrocarbons