GeoPT2. International Proficiency Test for Analytical Geochemistry Laboratories - Report on Round 2

Results from sixty laboratories participating in GeoPT2, the international proficiency testing programme for analytical geochemistry laboratories, are reported. Compared with 71.3% in the last round, 74.6% of the reported data complied with the laboratories' selected fitness for purpose criteria.     

GeoPT5. An International Proficiency Test for Analytical Geochemistry Laboratories - Report on Round 5

Results are presented from the seventy two laboratories participating in GeoPT5, round five of the international proficiency testing programme for analytical geochemistry laboratories. The sample for round five, AMH-1 (Mount Hood andesite), was distributed during March 1999 and participating laboratories were asked to analyse the sample using their routine techniques and submit results to the steering by 15th June 1999. In this report, contributed data are listed together with the derived z-scores from which participating laboratories can assess their analytical performance. Z-scores in the range -2 to 2 are considered satisfactory. Z-score values that lie outside this range may indicate unsuspected analytical bias. The distinctive feature of the present round is that AMH-1 is a candidate reference material prepared by the USGS and it is intended that the present proficiency testing data will contribute to the reference material characterisation programme.     

GeoPT4. An International Proficiency Test for Analytical Geochemistry Laboratories - Report on Round 4 (March 1999)

Results are presented from the seventy five laboratories participating in GeoPT4, round four of the international proficiency testing programme for analytical geochemistry laboratories. Laboratories were required to analyse the sample OU-2 (Belford dolerite) using routine methods of analysis. The sample was distributed during September 1998 with a deadline for the submission of results of 15th January 1999. In this report, contributed data are analysed and z-scores calculated. Z-score values provide participating laboratories with information concerning the quality of their results and indicate data that may be subject to unsuspected analytical bias. Laboratories are invited to examine these data and take the appropriate action.     

G-Probe-1 - An International Proficiency Test for Microprobe Laboratories - Report on Round 1 : February 2002 (TB-1 Basaltic Glass)

Results are presented for round one of a new international proficiency testing programme designed for microprobe laboratories involved in the routine analysis of silicate minerals. The sample used for this round was TB-1, a basaltic glass fused and prepared by the USGS. Thirty nine laboratories contributed data to this round, the majority of major element results being undertaken by EPMA and the majority of trace elements by LA-ICP-MS. Assigned values were derived from the median of results produced by nine selected laboratories that analysed powdered material by conventional ICP-MS, INAA and XRF techniques using bulk powders of the sample. Submitted microprobe results were evaluated using a target precision calculated using the Horwitz function, adopting the same criteria as those used for "applied" geochemistry laboratories in the companion GeoPT proficiency testing programme for laboratories involved in the routine bulk analysis of silicate rocks. An evaluation of results from participating microprobe laboratories indicated that overall, data were compatible with this precision function. A comparison between the performance of bulk and microprobe techniques used in the analysis of the basaltic glass showed remarkably good agreement, with significant bias only observed for the major oxide MgO.     

The GeoPT Proficiency Testing Scheme for Laboratories Routinely Analysing Silicate Rocks: A Review of the Operating Protocol and Proposals for its Modification

The GeoPT proficiency testing programme for geochemical laboratories has been operating for nearly 20 years. This review, based on an analysis of accumulated data and extensive experience, examines whether the protocol followed during this period continues to be appropriate. Possible changes that might be considered for future implementation are examined, in particular the procedures for calculating assigned values, target values, z‐scores and the applicability of dual fitness‐for‐purpose criteria. We conclude that the existing protocol remains largely appropriate and effective, but propose that a single fitness‐for‐purpose criterion be adopted, with an option for laboratories to recalculate their z‐scores if the criterion is inappropriate for their requirements.     

An Evaluation of Methods for Assessing the Competence of Laboratories Based on Performance in the GeoPT Proficiency Testing Scheme

The original certification protocol, published by the International Association of Geoanalysts in 2003, specified that the competence of laboratories selected as competent to contribute certification measurements should be evaluated from their performance in the GeoPT proficiency testing programme. Round 39 of the IAG GeoPT proficiency testing programme provided an opportunity to examine four methods of evaluating laboratory competence based largely on the use of proficiency testing z‐scores as performance indicators. This opportunity arose because two test materials were co‐analysed by participating laboratories in this round: a syenite, SyMP‐1, supplied by the USGS, and an established CRM, the nepheline syenite, CGL 006. The performance of laboratories was assessed in four ways; in each case, consensus values and their uncertainties as derived from selective data sets of competent laboratories were compared with results derived from the routine GeoPT data assessment, involving all submitted measurements. An overall comparison of results showed no significant statistical differences in either consensus values or uncertainties between these data sets. This conclusion was unexpected and calls into question the widely held assumption that ‘better’ consensus data would be obtained from a subset of laboratories judged to be competent on the basis of proficiency testing performance indicators.     

The GeoPT Proficiency Testing Programme as a Scheme for the Certification of Geological Reference Materials

ISO Guide 35:2017 provides, for the first time, an alternative way of characterising certified reference materials using proficiency testing. In this paper, the properties of assigned values derived from the well‐established GeoPT proficiency testing scheme are examined. This scheme, designed for laboratories that undertake the routine analysis of silicate rocks and related materials, routinely has over 100 participants contributing results. Following a detailed assessment of the metrological properties of GeoPT assigned values in relation to Guide 35 recommendations, it is demonstrated that these values may be regarded as certified values, provided a number of criteria are met. These criteria include the following: a demonstration of sufficient homogeneity of the candidate CRM; circulation, when judged to be appropriate, of an established matrix‐matched CRM for co‐analysis in that round; the robust statistical analysis of data sets using GeoPT established criteria; a decision whether assigning a value is justified (including a requirement of a minimum of fifteen valid results); and an expert group to manage the certification and the maintenance of appropriate records. In summary, the GeoPT proficiency testing scheme, subject to the arrangements summarised above, is considered to be competent for the certification of geological reference materials.     

The Long‐Term Robustness and Stability of Consensus Values as Composition Location Estimators for a Typical Geochemical Test Material in the GeoPT Proficiency Testing Programme

Re‐issuing the same test material, its true identity unknown to participants, in two rounds of the GeoPT proficiency testing programme 18 years apart has demonstrated remarkable similarity, and therefore stability, of consensus values independently estimated for over fifty measurands in each round. A comparison of the two data sets, GeoPT5 (AMH‐1) from 1999 and GeoPT41 (ORA‐1) from 2017, shows that corresponding consensus values, rigorously derived by current procedures for complete compatibility, are for the most part statistically indistinguishable when account is taken of their associated uncertainties. Inferences that may be drawn from this exceptional agreement include: (a) the consensus estimation procedure was robust and gave consistent results; (b) overall, the balance of the contributed data was unaffected by significant changes in: (i) the populations of laboratories participating, (ii) the proportions of laboratories producing results by different techniques, (iii) the manner in which systems were calibrated, or (iv) the aspirations of laboratories to attain higher quality results over time; and (c) unsurprisingly perhaps, that the test material itself had remained stable and unchanged during that time. Additionally, a statistical comparison of the original values for AMH‐1 with consensus values derived by current procedures demonstrates that they are also effectively indistinguishable.     

The Reliability of Assigned Values from the GeoPT Proficiency Testing Programme from an Evaluation of Data for Six Test Materials that have been Characterised as Certified Reference Materials

Assigned values derived from the GeoPT proficiency testing programme were compared with certified values for six certified reference materials that have been used as test materials in the GeoPT programme. Statistical analysis showed that there were few significant differences between these sets of data and that these differences had no significant impact on the GeoPT assessment when fitness‐for‐purpose criteria were taken into account.     

An Assessment of Performance in the Routine Analysis of Silicate Rocks Based on an Analysis of Data Submitted to the GeoPT Proficiency Testing Programme for Geochemical Laboratories (2001–2011)

Data reported by laboratories contributing to the GeoPT proficiency testing programme for geochemical laboratories over the period from 2001 to 2011 have been assessed to identify the elements and concentration ranges over which analytical performance can be considered satisfactory. Criteria developed in the paper indicated that performance in the content determination of the elements/constituents SiO₂, Al₂O₃, MnO, Cs, Dy, Er, Eu, Ga, Hf, Ho, Lu, Nd, Pr, Sm, Sr, Tb, Tl, Tm, U, Y, Yb and Zn was satisfactory over the full concentration range assessed. The elements/constituents TiO₂, Fe₂O₃(T), MgO, CaO, Na₂O, K₂O, P₂O₅, Ba, Be, Cd, Ce, Co, Gd, La, Li, Nb, Rb, Sb, Sc, Sn, Ta, Th, V and Zr showed some degradation in performance at lower concentration levels (approaching the detection limit of some techniques). Performance in determining LOI, As, Bi, Cr, Cu, Ge, Mo, Ni, Pb and W was in general unsatisfactory over the full concentration range assessed. Other elements (especially Fe(II)O, H₂O⁺, CO₂, Ag, Au, B, Br, Cl, F, Hg, I, In, Ir, N, Os, Pd, Pt, Re, Rh, S, Se, Te) could not be evaluated as they were not routinely reported by laboratories participating in the GeoPT programme, often because they are present in silicate rocks at sufficiently low concentrations to require a pre‐concentration stage. Some suggestions are made for the causes of unsatisfactory performance, but further progress will require a detailed assessment of the methods used by participating laboratories, which will form the subject of a further paper.     

超深地质钻孔的质量控制探讨——以磁西一号勘探区37—3孔为例

河北平原区找煤和老矿区外围勘探深度多在1500m左右,钻孔的质量控制成为保证勘查报告质量的关键。以磁西一号勘探区37—3孔为例,介绍了超深钻孔的的质量控制措施,指出了在孔斜预防方面,要求钻塔安装稳固．选择适宜的钻进参数,采用钻铤加压,保持钻具不弯曲,每200m进行测斜一次;在岩心采取方面,使用双管取心和岩心提断器进行取心,钻时控制在2．5～3h,进尺不超过3m,严格按比例配制泥浆;在采取煤心时,运用三层管单动取煤器取粉煤及块煤,伸缩式二型取煤器取易碎煤心的方法。通过对超深地质孔质量控制关键环节的分析,提出了对超深地质孔质量控制的方法和建议。