The determination of 52 elements in marine geological samples by an inductively coupled plasma optical emission spectrometry and an inductively coupled plasma mass spectrometry with a high-pressure closed digestion method

An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.

Effect of variety and drying method on the nutritive value of corn for growing pigs

Background：This experiment was conducted to determine the nutritive value of corn from the north of China for growing pigs.The experiment examined corn variety（LS1,LS2,LS3 and LS4）grown in one location,drying method（sun dried and artificially dried）and different drying temperatures.Corn harvested at 20-25%moisture was dried to about 12%moisture by sun drying and artificially drying at 80,100,or 120℃ in a fluidized bed dryer.Ninety-six barrows（average BW of 33.4 ± 2.7 kg）were housed in individual metabolism crates to facilitate separate collection of feces and urine.A five-day collection period followed a seven-day diet acclimation period.Results：The results indicated that variety significantly influenced（P〈0.01）the 1,000 kernel weight of corn but not the bulk weight.Variety also influenced the available energy content（digestible energy of dry matter,P〈0.01;metabolisable energy of dry matter,P〈0.01）and digestibility of organic matter（P〈0.01）,as well as dry matter（P〈0.01）and gross energy（GE）content（P〈0.02）.The drying method of corn significantly influenced the 1,000 kernel weight（P〈0.01）,bulk weight（P〈0.01）and digestibility of ether extract（EE）（P〈0.01）.No effect of drying temperature on the digestibility of organic matter,dry matter（DM）,crude protein（CP）,neutral detergent fiber（NDF）,acid detergent fiber（ADF）and gross energy was observed,but gelatinization（P〈0.05）and test weight（P〈0.01）decreased with an increase in temperature.Conclusions：Variety has a significant impact on the nutritive value of corn for growing pigs,and greater attention needs to be paid to these influences in the assignment of the nutritive value of corn given to growing pigs.

Methodological impact of starch determination on starch content and ileal digestibility of starch in grain legumes for growing pigs

Background： Grain legumes represent a valuable energy source in pig diets due to their high starch content. The present study was conducted to determine the content and apparent ileal digestibility（AID） of starch in different grain legume cultivars for pigs by means of both a polarimetric and enzymatic method for starch determination.Methods： Three experiments were conducted with six barrows each which were fitted with ileal T-cannulas. In total, 18 diets including six different cultivars of faba beans（Vicia faba L.） and peas（Pisum sativum L.）, five different cultivars of lupins（Lupinus luteus L., Lupinus angustifolius L.）, and one diet with a soybean meal（SBM） were fed.Results： The starch content of faba beans and peas was greater（P ＆lt; 0.05） when determined polarimetrically than enzymatically（438 vs. 345 g/kg dry matter（DM） in faba beans and 509 vs. 390 g/kg DM in peas, respectively）.Considerable lower starch contents were obtained in lupins and SBM, with 82 and 48 g/kg DM（analyzed polarimetrically） and ＆lt;1.1 and 3 g/kg DM（analyzed enzymatically）, respectively. Mean values for contents of neutral detergent fiber（NDF） and acid detergent fiber（ADF） in grain legumes ranged from 111 and 79 g/kg DM in peas to248 and 207 g/kg DM in lupins, respectively. Contents of condensed tannins in the colored flowered faba bean cultivars ranged from 2.1 to 7.4 g/kg DM. The AID of starch was greater（P ＆lt; 0.05） in pea than in faba bean cultivars,and using the polarimetric starch determination method resulted in greater（P ＆lt; 0.05） digestibility values than using enzymatic starch analysis（84 vs. 80% in faba beans and 86 vs. 83% in peas）. Moreover, AID of starch differed（P ＆lt; 0.05）within pea cultivars and starch digestibility in faba beans decreased linearly（P ＆lt; 0.05） as the content of condensed tannins increased. However, there was no relationship between contents of NDF and ADF and AID of starch in pea and faba bean cultivars.Conclusion： Both contents and AID of starch in grain legumes can vary as influenced by the analytical method used for starch determination. Generally, starch digestibility is greater when measured by polarimetric rather than enzymatic methods.

Rapid genetic screening of Charcot-Marie-Tooth disease type 1A and hereditary neuropathy with liability to pressure palsies patients

We used the allele-specific PCR-double digestion method on peripheral myelin protein 22 （PMP22） to determine duplication and deletion mutations in the proband and family members of one family with Charcot-Marie-Tooth disease type 1 and one family with hereditary neuropathy with liability to pressure palsies. The proband and one subclinical family member from the Charcot-Marie-Tooth disease type 1 family had a PMP22 gene duplication; one patient from the hereditary neuropathy with liability to pressure palsies family had a PMP22 gene deletion. Electron microscopic analysis of ultrathin sections of the superficial peroneal nerve from the two probands demonstrated demyelination and myelin sheath hyperplasia, as well as an ＇onion-like＇ structure in the Charcot-Marie-Tooth disease type 1A patient. We observed an irregular thickened myelin sheath and ＇mouse-nibbled＇-Iike changes in the patient with hereditary neuropathy with liability to pressure palsies. In the Charcot-Marie-Tooth disease type 1A patient, nerve electrophysiological examination revealed moderate-to-severe reductions in the motor and sensory conduction velocities of the bilateral median nerve, ulnar nerve, tibial nerve, and sural nerve. Moreover, the compound muscle action potential amplitude was decreased. In the patient with hereditary neuropathy with liability to pressure palsies, the nerve conduction velocity of the bilateral tibial nerve and sural nerve was moderately reduced, and the nerve conduction velocity of the median nerve and ulnar nerve of both upper extremities was slightly reduced.

Effect of the chlortetracycline addition method on methane production from the anaerobic digestion of swine wastewater

Effects of antibiotic residues on methane production in anaerobic digestion are commonly studied using the following two antibiotic addition methods：（1） adding manure from animals that consume a diet containing antibiotics, and（2） adding antibiotic-free animal manure spiked with antibiotics. This study used chlortetracycline（CTC） as a model antibiotic to examine the effects of the antibiotic addition method on methane production in anaerobic digestion under two different swine wastewater concentrations（0.55 and 0.22 mg CTC/g dry manure）. The results showed that CTC degradation rate in which manure was directly added at 0.55 mg CTC/g（HSPIKE treatment） was lower than the control values and the rest of the treatment groups. Methane production from the HSPIKEtreatment was reduced（p 〈 0.05） by 12% during the whole experimental period and 15% during the first 7 days. The treatments had no significant effect on the pH and chemical oxygen demand value of the digesters, and the total nitrogen of the0.55 mg CTC/kg manure collected from mediated swine was significantly higher than the other values. Therefore, different methane production under different antibiotic addition methods might be explained by the microbial activity and the concentrations of antibiotic intermediate products and metabolites. Because the primary entry route of veterinary antibiotics into an anaerobic digester is by contaminated animal manure, the most appropriate method for studying antibiotic residue effects on methane production may be using manure from animals that are given a particular antibiotic, rather than adding the antibiotic directly to the anaerobic digester.

Simple and cost-effective methods for precise analysis of trace element abundances in geological materials with ICP-MS

Inductively coupled plasma mass spectrometry （ICP-MS） is the most commonly used technique to deter- mine the abundances of trace elements in a wide range of geological materials. However, incomplete sample digestion, isobaric interferences and instrumental drift remain obvious problems that must be overcome in order to obtain precise and accurate results, For this reason, we have done many experi- ments and developed a set of simple, cost-effective and practical methods widely applicable for precise and rapid determination of trace element abundances in geological materials using ICP-MS. Commonly used high-pressure digestion technique is indeed effective in decomposing refractory phases, but this inevitably produces fluoride complexes that create new problems. We demonstrate that the fluoride complexes formed during high-pressure digestion can be readily re-dissolved using high-pressure vessel at 190 ℃ for only 2 h for 50 mg sample. In the case of isobaric interferences, although oxide （e.g., MO^＋/M^＋） and hydroxide （e.g., MO^＋/M^＋） productivity is variable between runs, the （MO^＋/M^＋）/（CeO^＋/Ce^＋） and （MOH^＋/M^＋）/（CeO^＋/Ce^＋） ratios remain constant, making isobaric interference correction for all other elements of interest straightforward, for which we provide an easy-to-use off-line procedure. We also show that mass-time-intensity drift curve is smooth as recognized previously, for which the correction can be readily done by analyzing a quality-control （QC） solution and using off-line Excel VBA procedure without internal standards. With these methods, we can produce data in reasonable agreement with rec- ommended values of international rock reference standards with a relative error of 〈8% and precision generally better than 5%. Importantly, compared to the widely used analytical practice, we can effectively save 〉60% of time （e.g., 〈24 h vs. 〉60 h）.

Fabrication of nano-sized Ca(OH)_2 with excellent adsorption ability for N_2O_4

Uniform nano-sized calcium hydroxide （Ca（OH）2） monocrystal powder was synthesized from calcium oxide in a surfactant solution via a digestion method by decreasing the surface tension of the reaction system to control the growth of crystalline Ca（OH）2. The Ca（OH）2 monocrystal powder samples were characterized by means of scanning electron microscopy （SEM）, transmission electron microscopy （TEM）, high resolution transmission electron microscopy （HRTEM）, X-ray diffraction （XRD）, Brunauer-Emmett-Teller （BET）, and Fourier transform-infrared spectroscopy （FT-IR）. The NOx adsorption ability of the samples was evaluated, and the influence of various types and concentrations of surfactants on powder agglomeration and then the specific surface area in the precipitation process were studied. The specific surface area of the samples was found as high as 58 m2/g and 92 m2/g and the particle size, 300-400 nm and 200-300 nm in the presence of 10 wt% PEG600 and 0.086 mL/L SDS at a reaction time of 5 h, respectively. The product has an exceptionally strong adsorption ability for NOx, which makes it a highly promising adsorbent for emission control and air purification.