CN109884036A - A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz - Google Patents

A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz Download PDF

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Publication number
CN109884036A
CN109884036A CN201910173910.2A CN201910173910A CN109884036A CN 109884036 A CN109884036 A CN 109884036A CN 201910173910 A CN201910173910 A CN 201910173910A CN 109884036 A CN109884036 A CN 109884036A
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China
Prior art keywords
quartz
ptfe
polytetrafluoroethylene
microelement
tungsten
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CN201910173910.2A
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Chinese (zh)
Inventor
李建德
王小虎
王曼丽
赵秀芳
张鹏
蒋丽薇
张意
徐艳艳
高丽荣
吴健蓉
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National Silicon Material Deep Processing Product Quality Supervision And Inspection Center East China Sea Research Institute
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National Silicon Material Deep Processing Product Quality Supervision And Inspection Center East China Sea Research Institute
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Priority to CN201910173910.2A priority Critical patent/CN109884036A/en
Publication of CN109884036A publication Critical patent/CN109884036A/en
Pending legal-status Critical Current

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Abstract

The present invention relates to a kind of sampling methods using microelement in inductively coupled plasma emission spectrography measurement quartz.Quartz is placed on self-control tungsten-molybdenum alloy plate, being tapped first with self-control tungsten-molybdenum alloy hammer keeps it broken, the preferably quartzy fragment of sizeable mass ratio is clamped with polytetrafluoroethylene (PTFE) clip again to be put into self-control tungsten grinding alms bowl, then continue to break into pieces and be ground to grinding rod sizeable powdered, finally take appropriate powder sample to be put into polytetrafluoroethylene (PTFE) counteracting tank with polytetrafluoroethylene (PTFE) spoon and carry out the analysis operation of lower step.Detection method sample processing time is short, and test result is accurate, reliable, can more embody the true value of microelement in quartz.

Description

Micro member in a kind of application inductive coupling plasma emission spectrograph measurement quartz The sampling method of element
Technical field
The present invention relates to analysis and testing technology fields, are related to a kind of application inductively coupled plasma emission spectrography survey Determine the sampling method of microelement in quartz.
Background technique
Microelement mainly applies inductive coupling plasma emission spectrograph to be analyzed in quartz at present.Wherein stone Diamond stone sampling method is broken into pieces after quartz is mainly printed blank sheet of paper package with common A4 with iron hammer, the quartz sand that then will be broken into pieces It is placed on the sieve of certain mesh number and sieves, the silica flour sieved is put into evaporating dish and is repeatedly rinsed with deionized water, is put into Drying in oven 4 hours, other analysis operations were carried out afterwards.Since the detection limit of microelement in quartz reaches mg/Kg grades, pole There is the distortion of result vulnerable to external pollution.
Since the hardness of quartz is 7 and quality is hard, and the hardness of common iron hammer is lower than 7 and quality is soft, thus with Iron hammer inevitably can occupy iron filings on the surface of quartz sand when tapping, and be difficult letter with this iron filings being adhered to above quartz sand It is applied alone deionized water to rinse well.
If it is also possible to remaining shredded paper, cannot guarantee that and rinsed well with deionized water inside the quartz sand broken into pieces, It is more serious to the damage ratio of the conventional elements such as potassium, sodium, it is also difficult to be rinsed well with deionized water.Besides sieve itself is metal Silk establishment, and sieve itself is also cleared up not completely, and the residual of sample can bring pollution to sample is being analyzed.
Traditional sampling method can seriously affect micro- in Inductively coupled plasma optical emission spectrometer analysis quartz in summary The authenticity of secondary element result, false testing result serious person are possible to that serious warp can be brought to quartz sand manufacturing enterprise Ji loss.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of application inductively coupled plasma emission spectrographies to measure stone The sampling method of microelement in diamond stone, to improve reliability, the accuracy of testing result.
The present invention is that technical solution used by solving its technical problem is:
1, a kind of sampling method using micro impurity element in inductive coupling plasma emission spectrograph analysis quartz, packet Include following steps:
(1) quartz is placed on self-control tungsten-molybdenum alloy plate, being tapped with self-control tungsten-molybdenum alloy hammer keeps it broken;
(2) the preferably quartzy fragment of sizeable mass ratio is clamped with polytetrafluoroethylene (PTFE) clip be put into self-control tungsten grinding alms bowl In, continue to break into pieces and be ground to grinding rod sizeable powdered;
(3) it takes appropriate powder sample to be put into polytetrafluoroethylene (PTFE) counteracting tank with polytetrafluoroethylene (PTFE) spoon and carries out lower step analysis operation.
2, compared with prior art, the present invention has following clear advantage:
(1) present invention sufficiently analyzes client to the statistics of the normal demand type of quartz microelement, finds to tungsten and two kinds of molybdenum The no demand of the analysis of element, so not having to consider pollution of the tungsten to sample in sampling process;
(2) quartzy hardness is 7 or so and quality is crisp, and the hardness of tungsten-molybdenum alloy is up to 20 or more and hard, uses tungsten Alloy is easy to quartz to break into pieces, does not have the surface that tungsten clast is adhered to quartz gravel, so not having to consider tungsten Influence of the element to test result;
(3) present invention does not have to sieve, avoids pollution of the residual of sieve itself and other samples to sample;
(4) this method does not need to rinse using deionized water, dries without baking oven, so shortening the sample preparation time, reduces The time of entire testing process, detection efficiency is improved, the probability that external environment pollutes sample is reduced.
Specific embodiment
Following non-limiting embodiments can with a person of ordinary skill in the art will more fully understand the present invention, but not with Any mode limits the present invention.
Embodiment 1
1,2,3,4, No. 5 each two parts of quartz are taken, a copy of it is placed on iron plate after being wrapped with common A4 printing paper, is struck with iron hammer It is broken, it pours into sieve and is sieved, the quartz sand of sieving stays on A4 paper, pours into evaporating dish, and baking is put into after being cleaned with deionized water It is dried in case, following steps are in strict accordance with microelement in laboratory inductive coupling plasma emission spectrograph measurement quartz Method carry out operation and upper machine analyze, obtain test result 1.Another is handled using this method, first with self-control tungsten hammer certainly It is knocked open on tungsten plate processed, then knocks high-quality quartz gravel open with one piece of the clamping of polytetrafluoroethylene (PTFE) clip and be put into self-control tungsten conjunction In gold grinding alms bowl, finally continues to break quartz gravel into pieces with tungsten-molybdenum alloy grinding rod and be ground into the suitable powder of granular size, with Lower step is carried out in strict accordance with the method for microelement in laboratory inductive coupling plasma emission spectrograph measurement quartz It operates and upper machine is analyzed, obtain test result 2.The common elements test result comparison that corresponding two kinds of method for making sample analyze is shown in Table 1.
1 quartz sample common elements test data result table of table
Obtain the value of microelement in quartz than the quartz that conventional method obtains using the method for the present invention as can be seen from Table 1 The value of microelement is generally wanted small in stone, it was demonstrated that and detection method sample processing time is short, and test result is accurate, reliable, The true value of microelement in quartz can more be embodied.

Claims (4)

1. a kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz, feature It is to include the following steps:
(1) quartz is placed in alloy sheets, being tapped with alloy hammer keeps it broken;
(2) it is put into grinding alms bowl, is used positioned at the preferable fragment disease of mass ratio in quartz fragment with clip clamping is sizeable Grinding rod continues to break quartz wedge into pieces and is ground to the suitable powder of granular size;
(3) it takes appropriate quartz powder to be put into polytetrafluoroethylene (PTFE) counteracting tank with spoon, carries out next step analysis step behaviour.
2. the method according to claim 1, which is characterized in that alloy sheets described in step (1) are self-control tungsten-molybdenum alloy Plate, alloy hammer are that tungsten-molybdenum alloy is hammered into shape.
3. the method according to claim 1, which is characterized in that clip described in step (2) is polytetrafluoroethylene (PTFE) clip, Grinding alms bowl is that self-control tungsten-molybdenum alloy grinds alms bowl, and grinding rod is tungsten-molybdenum alloy grinding rod.
4. the method according to claim 1, which is characterized in that clip described in step (3) is polytetrafluoroethylene (PTFE) clip.
CN201910173910.2A 2019-03-08 2019-03-08 A kind of sampling method using microelement in inductive coupling plasma emission spectrograph measurement quartz Pending CN109884036A (en)

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CN109142018A (en) * 2018-07-12 2019-01-04 昆山鸿福泰环保科技有限公司 A kind of method of the quick measurement containing rhodium content in rhodium material

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