CN101303308A - Method for measuring beryllium and compounds in the air of industry location - Google Patents

Method for measuring beryllium and compounds in the air of industry location Download PDF

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Publication number
CN101303308A
CN101303308A CNA2008100397947A CN200810039794A CN101303308A CN 101303308 A CN101303308 A CN 101303308A CN A2008100397947 A CNA2008100397947 A CN A2008100397947A CN 200810039794 A CN200810039794 A CN 200810039794A CN 101303308 A CN101303308 A CN 101303308A
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beryllium
air
sample
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concentration
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宋薇
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SHANGHAI PONY TESTING TECHNOLOGY Co Ltd
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SHANGHAI PONY TESTING TECHNOLOGY Co Ltd
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Abstract

The invention relates to a measurement method for beryllium and compound thereof in an atmosphere of industrial sites, which uses an inductively coupled plasma atomic emission spectrometry for detection, which is convenient, reliable, overcoming the defect of complex operation of the prior morin fluorescence spectrophotometry meeting the need of detection practice and research. The invention fills the blank of using the inductively coupled plasma atomic emission spectrometry (ICP-AES) for beryllium and compound detection in an atmosphere of industrial sites.

Description

The assay method of beryllium and compound thereof in the air of industry location
Technical field
The present invention relates to the assay method of beryllium in the air of industry location and compound thereof.
Background technology
Beryllium and compound thereof be severe toxicity all, and flue dust, the steam of contact beryllium or solubility beryllium salt can cause diseases such as dermatitis ulcer, upper respiratory tract pathology, berylliosis of lung, and beryllium almost all is absorbed after entering human body, can cause death when concentration is high.Beryllium is also classified as one of important carcinogenic substance by U.S. EPA.Though present national occupational health standard adopts the sensitivity of morin fluorescence spectrophotometry higher, complex operation, the time of preparation sample is long, and the sample solution stabilization time for preparing is within an hour, and adding reagent is more, and experimental cost is higher relatively.
Summary of the invention
Purpose of the present invention is exactly the defective that overcomes complex operation that existing morin fluorescence spectrophotometry exists etc., and the assay method of a kind of beryllium easy and simple to handle, reliable and compound thereof is provided.
The assay method of beryllium and compound thereof in the air of industry location of the present invention is to utilize ICP-AES (ICP-AES) to detect.
The assay method of beryllium and compound thereof in the above-mentioned air of industry location, its concrete steps are as follows:
The sampling that a, use install miillpore filter is clipped in sampled point collection air sample;
B, handle sample, use the dissolving with hydrochloric acid residue then, quantitatively be transferred in the color-comparison tube for measuring, if beryllium concentration surpasses measurement range in the sample liquid, with the hydrochloric acid solution dilution back mensuration of same concentration with digestive juice;
The drafting of c, typical curve: in a plurality of volumetric flasks, add the beryllium standard solution respectively, be made into the standard series of beryllium content with same concentration hydrochloric acid solution dilution, measure each standard series with inductive coupling plasma emission spectrograph then, with the spectral intensity average to beryllium concentration drawing standard curve;
D, with the operating conditions working sample and the blank solution of bioassay standard series, the sample spectra intensity that records deducted the spectral intensity of blank after, get the concentration of beryllium by typical curve.
The assay method of beryllium and compound thereof in the above-mentioned air of industry location, sample collecting among the step a wherein can be divided three kinds: short time sampling, sampling and personal sampling for a long time.
Short time sampling: at sampled point, with installing the sampling folder of miillpore filter, with 3-7L/min flow collection 15-20min air sample.
Long-time sampling: at sampled point, with installing the small plastic sampling folder of miillpore filter, with 1-3L/min flow collection 2～8h air sample.
Personal sampling: the small plastic sampling folder that will install miillpore filter is worn on the top, shirtfront of monitoring target, and air intake opening is as far as possible near breathing, band, with 1-3L/min flow collection 2～8h air sample.After the sampling, with filter membrane connect dirt face in doubling 2 times, put into cleaning polybag or paper bag, place in the container of cleaning transportation and preserve.At room temperature, but the sample long preservation.
The assay method of beryllium and compound thereof in the above-mentioned air of industry location, wherein among the step b to the processing of sample, its reagent all adopts standard inventory solution (supervise at national standard material center), nitric acid (top grade is pure); High-purity argon gas (〉=99.999%).
The concrete grammar of sample preparation is: the filter membrane that will adopt sample is put into beaker, add 5～10ml digestive juice, both the perchloric acid of 1+9-nitric acid acid mixture heated on electric hot plate and cleared up, maintain the temperature at about 200 ℃, treat that digestive juice volatilizees when doing substantially, take off cold slightly after, with 0.6mol/L dissolve with hydrochloric acid solution residue, quantitatively be transferred in the color-comparison tube, and be diluted to 10.0ml, shake up, for measuring.If beryllium concentration surpasses measurement range in the sample liquid, measure with 0.6mol/L hydrochloric acid solution dilution back, multiply by extension rate during calculating.
The assay method of beryllium and compound thereof in the above-mentioned air of industry location, wherein the blank sample of step c is that the sampling that installs miillpore filter is carried secretly to sampled point, gather the air sample except that not connecting air sampler, all the other operate same sample, as the blank of sample.
One of method for drafting of typical curve: in 6 10ml volumetric flasks, add 0.00,0.20,0.30,0.40,0.50 respectively, 0.60ml beryllium standard solution (0.10 μ g/mL), end scale with the dilution of 0.6mol/L hydrochloric acid solution, be made into the standard series of 0.000,0.002,0.003,0.004,0.005,0.006 μ g/mL beryllium content.Inductive coupling plasma emission spectrograph is adjusted to the optimum determining state, measures each standard series; Each concentration replication 3 times, with the spectral intensity average to beryllium concentration (μ g/mL) drawing standard curve.Coefficient R＞0.9990.
Used analytical instrument can adopt the thermoelectric ICP-AES of the U.S..The better detecting condition is as follows:
Emission wavelength: 313.042nm;
Incident power: 1150W;
Atomizer pressure: 0.18MPa;
Secondary air amount: 0.5L/min;
Observed altitude: 10mm;
Pump speed: 50rpm
Beryllium and compound concentration computing formula thereof in the last workplace:
By formula (1) sampling volume is converted into the standard sample volume:
Vo = V × 293 273 + t × P 101.3 · · · · · · ( 1 )
In the formula: Vo-standard sample volume, L;
The V-sampling volume, L;
The temperature of t-sampled point, ℃;
The atmospheric pressure of P-sampled point, kPa.
Calculate the concentration of beryllium in the air by formula (2):
C = 10 m Vo · · · · · · ( 2 )
In the formula: the concentration of beryllium in the C-air, mg/m 3
M-records the content of beryllium in the sample solution, μ g/mL;
Vo-standard sample volume, L.
Beneficial effect of the present invention: the method that is used for detecting beryllium in the air of industry location and compound thereof with ICP-AES (ICP-AES), convenient, reliable, overcome the defectives such as complex operation that existing morin fluorescence spectrophotometry exists.Though present national occupational health standard adopts the sensitivity of morin fluorescence spectrophotometry higher, complex operation, the time of preparation sample is long, and the sample solution stabilization time for preparing is within an hour, and adding reagent is more, and experimental cost is higher relatively.And use detection method of the present invention, easy to operate, the time of preparation sample is short, be 4 hours the sample solution stabilization time after the processing, the sample pretreatment process is simple relatively, more has superiority for the analysis of a large amount of samples, has satisfied people's testing and research needs.In addition, the method blank that ICP-AES (ICP-AES) is measured beryllium in the air of industry location and compound thereof has been filled up in the application of detection method of the present invention.
Description of drawings
The beryllium typical curve (Be313.042nm) that Fig. 1 is drawn in the sampling of forging and pressing workshop short time for embodiment 1.
The beryllium typical curve (Be313.042nm) that Fig. 2 is drawn in the long-time sampling in forging and pressing workshop for embodiment 2.
Embodiment
Embodiment 1
Beryllium assay in the short time sampling forging and pressing workshop air
1 forging and pressing workshop sampled point (temperature: 28 ℃, air pressure: 100.3kPa), will install the sampling folder of miillpore filter, on filter membrane 1#, the filter membrane 1# that adopted sample is put into beaker with 5L/min flow collection 15min air sample, add 5～10ml digestive juice, maintain the temperature at about 200 ℃ and clear up, treat that digestive juice volatilizees when doing substantially, take off cold slightly after, with 0.6mol/L dissolve with hydrochloric acid solution residue, quantitatively be transferred in the color-comparison tube, and be diluted to 10.0mL, shake up, for measuring.Getting blank filter membrane 0# and 1# filter membrane simultaneously handles with process.If beryllium concentration surpasses measurement range in the sample liquid, measure with 0.6mol/L hydrochloric acid solution dilution back, multiply by extension rate during calculating.
2 instruments: the thermoelectric ICP-AES of the U.S.
3 testing conditions:
Emission wavelength: 313.042nm;
Incident power: 1150W;
Atomizer pressure: 0.18MPa
Secondary air amount: 0.5L/min;
Observed altitude: 10mm
Pump speed: 50rpm
4.1 calculate the concentration of beryllium in the air by analytical procedure 5.1 Chinese styles (1), 5.2 Chinese styles (2):
4.2 precision and accuracy
4.2.1 precision
Sample replication result
Filter membrane 1# 1#-1 1#-2 1#-3 1#-4 1#-5 RSD/ ％
Beryllium (mg/m 3) 0.000726 0.000719 0.000710 0.000703 0.000714 1.26
4.2.2 accuracy
In order further to investigate the accuracy of this method, carry out mark-on with pure standard solution respectively and reclaim experiment.The actual sample recovery meets laboratory constant, microanalysis requirement between 94%～98%.
The mark-on sample of gathering is carried out repetition measure for 10 times, the recovery of standard addition result is as follows:
Sample Sample determination value mg/L Mark-on sample determination value mg/L Add standard volume μ g The recovery, %
The 1st time 0.00525 0.01005 0.050 96.0
The 2nd time 0.0052 0.00990 0.050 94.0
The 3rd time 0.00513 0.00987 0.050 94.8
The 4th 0.00508 0.00984 0.050 95.2
The 5th 0.00516 0.00998 0.050 96.4
The 6th time 0.00519 0.01005 0.050 97.2
The 7th time 0.00523 0.01004 0.050 96.2
The 8th time 0.00512 0.00985 0.050 94.6
The 9th time 0.00525 0.01002 0.050 95.4
The 10th time 0.00521 0.01004 0.050 96.6
4.3 optimization spectral line
By the RF power to instrument, parameters such as secondary air amount, atomizer pressure, observed ray are optimized, and selected RF power is 1150W, and atomizer pressure is 0.18MPa, and the secondary air amount is 0.5L/min.Can obtain analytical performance preferably with this understanding.
Select highly sensitive, disturb less, spectral line that the background equipotent concentration is low is as analytical line, therefore selects Be313.042nm.
Wavelength Interference element Intensity
313.042nm Ce 30000
234.861nm Ni，Mo 25000
313.107nm Th，Nb，Tm 25000
4.4 working curve and linear graph:
Be 313.042nm spectral intensity
0.000μg/mL 0
0.002μg/mL 122
0.003μg/mL 188
0.004μg/mL 244
0.005μg/mL 310
0.006μg/mL 370
Numbering Concentration (μ g/mL)
blank-1 0.0003
blank-2 0.0001
be-1 0.00525
be-2 0.0052
be-3 0.00513
be-4 0.00508
be-5 0.00516
average 0.005165
SD 0.0000582
RSD 0.011262761
Embodiment 2
Beryllium assay in the long-time collection beryllium-bronze workshop air
1 beryllium-bronze workshop air sampled point (temperature: 29 ℃, air pressure: 99.8kPa), will install the small plastic sampling folder of miillpore filter, with 1L/min flow collection 2h air sample on the 1# filter membrane.The filter membrane 1# that adopted sample is put into beaker, add 5～10mL digestive juice, maintain the temperature at about 200 ℃ and clear up, treat that digestive juice volatilizees when doing substantially, take off cold slightly after, with 0.6mol/L dissolve with hydrochloric acid solution residue, quantitatively be transferred in the color-comparison tube, and be diluted to 10.0mL, shake up, for measuring.Getting blank filter membrane 0# and 1# filter membrane simultaneously handles with process.If beryllium concentration surpasses measurement range in the sample liquid, measure with 0.6mol/L hydrochloric acid solution dilution back, multiply by extension rate during calculating.
2 instruments: the thermoelectric ICP-AES of the U.S.
3 testing conditions:
Emission wavelength: 313.042nm;
Incident power: 1150W;
Atomizer pressure: 0.18MPa
Secondary air amount: 0.5L/min;
Observed altitude: 10mm
Pump speed: 50rpm
4.1 calculate the concentration of beryllium in the air by analytical procedure 5.1 Chinese styles (1), 5.2 Chinese styles (2):
4.2 precision and accuracy
4.2.1 precision
Sample replication result
Filter membrane 1# 1#-1 1#-2 1#-3 1#-4 1#-5 RSD/％
Beryllium (mg/m 3) 0.000632 0.000656 0.000641 0.000649 0.000654 1.51
4.2.2 accuracy
In order further to investigate the accuracy of this method, carry out mark-on with pure standard solution respectively and reclaim experiment.The actual sample recovery meets laboratory constant, microanalysis requirement between 93%～102%.
The mark-on sample of gathering is carried out repetition measure for 10 times, the recovery of standard addition result is as follows:
Sample Sample determination value mg/L Mark-on sample determination value mg/L Add standard volume μ g The recovery, %
The 1st time 0.00725 0.01484 0.080 94.9
The 2nd time 0.00752 0.01530 0.080 97.3
The 3rd time 0.00735 0.01496 0.080 95.1
The 4th 0.00744 0.01554 0.080 101.3
The 5th 0.00750 0.01525 0.080 96.9
The 6th time 0.00741 0.01488 0.080 93.4
The 7th time 0.00751 0.01505 0.080 94.2
The 8th time 0.00745 0.01510 0.080 95.6
The 9th time 0.00737 0.01511 0.080 96.8
The 10th time 0.00753 0.1512 0.080 94.9
4.3 optimization spectral line
By the RF power to instrument, parameters such as secondary air amount, atomizer pressure, observed ray are optimized, and selected RF power is 1150W, and atomizer pressure is 0.18MPa, and the secondary air amount is 0.5L/min.Can obtain analytical performance preferably with this understanding.
Select highly sensitive, disturb less, spectral line that the background equipotent concentration is low is as analytical line, therefore selects Be313.042nm.
Wavelength Interference element Intensity
313.042nm Ce 30000
234.861nm Ni，Mo 25000
313.107nm Th，Nb，Tm 25000
Select 313.042nm, the intensity height, interference element is less.
4.4 working curve and linear graph:
Be 313.042nm spectral intensity
0.000μg/mL 0
0.002μg/mL 130
0.003μg/mL 199
0.004μg/mL 258
0.005μg/mL 320
0.006μg/mL 387
Numbering blank-1 Concentration (μ g/mL) 0.0002
blank-2 0.0001
be-1 0.00725
be-2 0.00752
be-3 0.00735
be-4 0.00744
be-5 0.00750
average 0.007412
SD 0.00010028
RSD 0.013529359

Claims (9)

1, the assay method of beryllium and compound thereof in the air of industry location is characterized in that: utilize ICP-AES to detect.
2, the assay method of beryllium and compound thereof in the air of industry location as claimed in claim 1, it is characterized in that: the testing conditions of the ICP-AES analytical instrument of use is: emission wavelength 313.042nm, incident power 1150W, atomizer pressure 0.18MPa, secondary air amount 0.5L/min, observed altitude 10mm, pump speed 50rpm.
3, the assay method of beryllium and compound thereof in the air of industry location as claimed in claim 1, it is characterized in that: concrete operation steps is as follows:
The sampling that a, use install miillpore filter is clipped in sampled point collection air sample;
B, handle sample, use the dissolving with hydrochloric acid residue of suitable concn then, quantitatively be transferred in the color-comparison tube for measuring, if beryllium concentration surpasses measurement range in the sample liquid, with the hydrochloric acid solution dilution back mensuration of same concentration with digestive juice;
The drafting of c, typical curve: in a plurality of volumetric flasks, add the beryllium standard solution respectively, be made into the standard series of different beryllium concentration with same concentration hydrochloric acid solution dilution, measure each standard series with inductive coupling plasma emission spectrograph then, with the spectral intensity average to beryllium concentration drawing standard curve;
D, with the operating conditions working sample and the blank solution of bioassay standard series, the sample spectra intensity that records deducted the spectral intensity of blank after, get the concentration of beryllium by typical curve.
4, the assay method of beryllium and compound thereof in the air of industry location as claimed in claim 3 is characterized in that: step a takes the short time sampling, promptly at sampled point, with installing the sampling folder of miillpore filter, with 3-7L/min flow collection 15-20min air sample.
5, the assay method of beryllium and compound thereof in the air of industry location as claimed in claim 3, it is characterized in that: step a takes long-time sampling, promptly at sampled point, with installing the small plastic sampling folder of miillpore filter, with 1-3L/min flow collection 2～8h air sample.
6, the assay method of beryllium and compound thereof in the air of industry location as claimed in claim 3, it is characterized in that: step a takes personal sampling, the small plastic sampling folder that is about to install miillpore filter is worn on the top, shirtfront of monitoring target, air intake opening is near breathing zone, with 1-3L/min flow collection 2～8h air sample.
7, the assay method of beryllium and compound thereof in the air of industry location as claimed in claim 3, it is characterized in that: the digestive juice that step b uses is the acid mixture of perchloric acid-nitric acid, dissolving postdigestive residue concentration of hydrochloric acid is 0.6mol/L.
8, the assay method of beryllium and compound thereof in the air of industry location as claimed in claim 3, it is characterized in that: the concrete method for drafting of step c typical curve is: in 6 10ml volumetric flasks, add 0.00,0.20,0.30,0.40,0.50 respectively, 0.60ml beryllium standard solution (0.10 μ g/mL), end scale with the dilution of 0.6mol/L hydrochloric acid solution, be made into the standard series of 0.000,0.002,0.003,0.004,0.005,0.006 μ g/mL beryllium content; Inductive coupling plasma emission spectrograph is adjusted to the optimum determining state, measures each standard series; Each concentration replication 3 times, with the spectral intensity average to beryllium concentration (μ g/mL) drawing standard curve; Coefficient R＞0.9990.
9, the assay method of beryllium and compound thereof in the air of industry location as claimed in claim 1 is characterized in that: beryllium and compound concentration computing formula thereof are as follows in the last workplace:
By formula (1) sampling volume is converted into the standard sample volume:
Vo = V × 293 273 + t × P 101.3 · · · · · · ( 1 )
In the formula: Vo-standard sample volume, L;
The V-sampling volume, L;
The temperature of t-sampled point, ℃;
The atmospheric pressure of P-sampled point, kPa
Calculate the concentration of beryllium in the air by formula (2):
C = 10 m Vo · · · · · · ( 2 )
In the formula: the concentration of beryllium in the C-air, mg/m 3
M-records the content of beryllium in the sample solution, μ g/mL;
Vo-standard sample volume, L.
CNA2008100397947A 2008-06-30 2008-06-30 Method for measuring beryllium and compounds in the air of industry location Pending CN101303308A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101556231B (en) * 2009-05-27 2011-01-05 谱尼测试科技（北京）有限公司 Ocean air salinity measuring method
CN104215630A (en) * 2013-11-12 2014-12-17 张文知 Method for rapidly measuring beryllium in mineral rocks
CN105738346A (en) * 2014-12-10 2016-07-06 上海宝钢工业技术服务有限公司 Method for determining content of boron and compounds thereof in air of workplace
CN107870167A (en) * 2016-09-27 2018-04-03 上海宝钢工业技术服务有限公司 The assay method of beryllium and its compound concentration in workplace air
CN108445061A (en) * 2018-03-19 2018-08-24 广东华晟安全职业评价有限公司 Tin and its assay method of compound in a kind of detection air
CN110361376A (en) * 2019-06-27 2019-10-22 上海宝钢工业技术服务有限公司 The measuring method of zirconium and its compound in workplace air

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101556231B (en) * 2009-05-27 2011-01-05 谱尼测试科技（北京）有限公司 Ocean air salinity measuring method
CN104215630A (en) * 2013-11-12 2014-12-17 张文知 Method for rapidly measuring beryllium in mineral rocks
CN105738346A (en) * 2014-12-10 2016-07-06 上海宝钢工业技术服务有限公司 Method for determining content of boron and compounds thereof in air of workplace
CN107870167A (en) * 2016-09-27 2018-04-03 上海宝钢工业技术服务有限公司 The assay method of beryllium and its compound concentration in workplace air
CN108445061A (en) * 2018-03-19 2018-08-24 广东华晟安全职业评价有限公司 Tin and its assay method of compound in a kind of detection air
CN108445061B (en) * 2018-03-19 2020-10-02 广东华晟安全职业评价有限公司 Determination method for detecting tin and compounds thereof in air
CN110361376A (en) * 2019-06-27 2019-10-22 上海宝钢工业技术服务有限公司 The measuring method of zirconium and its compound in workplace air

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Open date: 20081112